24小时热门版块排行榜    

查看: 1272  |  回复: 5

caijacky0912

木虫 (正式写手)

[求助] 求助埃索美拉唑钠的旋光值

请教一下,谁能查到埃索美拉唑钠的旋光数据啊?只要有的都可以,谢谢!
回复此楼
已阅   回复此楼   关注TA 给TA发消息 送TA红花 TA的回帖

hardee

铁杆木虫 (知名作家)

此草有主~

【答案】应助回帖

★ ★ ★ ★ ★ ★ ★
感谢参与,应助指数 +1
caijacky0912: 金币+5, ★★★很有帮助 2012-11-12 08:23:48
古可ぷ: 金币+2, 谢谢应助 2012-11-12 22:39:20
古可ぷ: 回帖置顶 2012-11-12 22:39:24
EP1515963
Example 4
Preparation of (-)-5-Methoxy-2-[[4-methoxy-3,5-dimethyl-2- pyridinyl) methyl]sulphinyl]-1H-benzimidazole Sodium Trihydrate Salt
Sodium hydroxide flakes (4.5 grams) were added to methanol (50 ml) and stirred for 15-30 minutes. The mass was cooled to a temperature of 5-10°C, esomeprazole obtained as in Example 2 (25.0 grams), and methanol (100.0 ml) were added with stirring for 30-60 minutes. The solvent was expelled off completely from the reaction solution. Di-isopropyl ether (150 ml) was added to the residual mass and further stirred for 30-60 minutes. The mass was cooled to a temperature of 0-5°C and stirred for 30-60 minutes to separate the solid mass. The solid mass was filtered and dried at a temperature of 60-70°C under vacuum to afford optically pure Esomeprazole Sodium trihydrate salt. The characteristics of the product are as follows. Weight: 14.5 g.
Chiral Purity: 99.53 Optical rotation: + 42° (c = 0.5% water)
安得促膝,可共平生。
2楼2012-11-10 09:49:31
已阅   回复此楼   关注TA 给TA发消息 送TA红花 TA的回帖

caijacky0912

木虫 (正式写手)

引用回帖:
2楼: Originally posted by hardee at 2012-11-10 09:49:31
EP1515963
Example 4
Preparation of (-)-5-Methoxy-2--1H-benzimidazole Sodium Trihydrate Salt
Sodium hydroxide flakes (4.5 grams) were added to methanol (50 ml) and stirred for 15-30 minutes. The ma ...

这个是三水的,有没有不带水的?或者其他带水的结晶数值啊?谢谢
3楼2012-11-12 11:55:04
已阅   回复此楼   关注TA 给TA发消息 送TA红花 TA的回帖

hardee

铁杆木虫 (知名作家)

此草有主~

★ ★ ★ ★ ★
古可ぷ: 回帖置顶 2012-11-12 22:39:57
古可ぷ: 金币+5, 谢谢帮助,欢迎常来 2012-11-12 22:40:08
United States Patent Application 20070259921  POLYMORPHIC FORMS OF ESOMEPRAZOLE SODIUM
这篇专利也有埃索钠不同晶型的介绍,其中有比旋度,但未指明溶液浓度,应该是差不多的:

Preparation of Crystalline Esomeprazole Sodium Form J
50 ml of methanol was taken into a round bottom flask and a mixture of 12.75 g sodium hydroxide and 11 ml of water was added to it and stirred for clear dissolution at 31° C. 110 g of esomeprazole was dissolved in 550 ml of methanol and the solution was added to the above methanolic sodium hydroxide solution. The mass was subjected to stirring at a temperature of 30° C. for 40 minutes, followed by the addition of 5.5 g of carbon with simultaneous stirring. The reaction mass was filtered through a Celite bed, and washed with 550 ml of methanol. The filtrate was subjected to distillation at a temperature of 30° C. under a vacuum of 200 torr. The residue was co-distilled with 1650 ml of acetone in three equal lots at 35° C. To the obtained residue, 220 ml of acetone was added and stirred for one hour. The separated solid was filtered and dried at 34° C. for 12 hours to afford 61.5 g of the title compound.

Moisture content: 1.35% w/w.

Specific optical rotation [α]D20=+43.220.

Purity by HPLC 99.99%.

Particle size distribution: D10 less than 3 μm, D50 less than 10 μm, D90 less than 30 μm.

Bulk density: Before tapping: 0.428 g/ml.

After tapping: 0.630 g/ml.

EXAMPLE 2
Preparation of Crystalline Esomeprazole Sodium Form K
11.1 g of esomeprazole and 50 ml of methanol were taken in to a round bottom flask and stirred for 15 minutes. 1.0 g of carbon was added to the reaction mass and subjected to stirring for 30 minutes followed by filtration of the reaction mass through a Hyflow (flux calcined diatomaceous earth) bed. The filter bed was washed with 30 ml of methanol. The filtrate was transferred into a round bottom flask and stirred. 6 ml of aqueous sodium hydroxide was added to the filtrate and stirred for 40 minutes. Then the reaction mass was subjected to distillation under a vacuum of 100 torr at a temperature of 30° C. for 1 hour. The obtained residue was co-distilled with 150 ml of acetone in three equal lots under a vacuum of 200 torr and a temperature of 30° C. The residue obtained was taken into 200 ml of acetone and stirred for 30 minutes. The separated solid was filtered and washed with 20 ml of acetone. The wet solid was dried at a temperature of 34° C. for 7 hours to afford 54.5 g of the title compound.

Moisture content: 8.87% w/w.

Specific optical rotation: [α]D20=+41.32°.

» 本帖已获得的红花(最新10朵)

安得促膝,可共平生。
4楼2012-11-12 12:44:06
已阅   回复此楼   关注TA 给TA发消息 送TA红花 TA的回帖

caijacky0912

木虫 (正式写手)

送鲜花一朵
引用回帖:
4楼: Originally posted by hardee at 2012-11-12 12:44:06
United States Patent Application 20070259921  POLYMORPHIC FORMS OF ESOMEPRAZOLE SODIUM
这篇专利也有埃索钠不同晶型的介绍,其中有比旋度,但未指明溶液浓度,应该是差不多的:

Preparation of Crystallin ...

非常感谢!
5楼2012-11-12 21:11:00
已阅   回复此楼   关注TA 给TA发消息 送TA红花 TA的回帖

acho-冰蝴蝶

新虫 (小有名气)

+28~+32
蝶恋花,花却随风摆……
6楼2014-10-16 19:56:29
已阅   回复此楼   关注TA 给TA发消息 送TA红花 TA的回帖
相关版块跳转 我要订阅楼主 caijacky0912 的主题更新
最具人气热帖推荐 [查看全部] 作者 回/看 最后发表
[基金申请] 欢迎发来filecode的Mz6后的代码验证其规律 +31 医学老男孩 2026-08-13 69/3450 2026-08-16 00:16 by mo_mo_mo_mo
[基金申请] filecode=后面第一个是大写字母 +6 wangze12014 2026-08-14 7/350 2026-08-15 20:12 by gltch
[基金申请] 小木虫上这么多卖论文的,真有人买论文么?感觉没必要啊 +12 Tide man 2026-08-10 13/650 2026-08-15 16:34 by 氺木
[基金申请] 哪位老哥知道今年的国自然具体哪一天放榜? +7 Ldrop2023 2026-08-13 7/350 2026-08-15 15:57 by mzhh2000
[基金申请] 关于Filecode分析方法 +10 majunge000 2026-08-10 13/650 2026-08-15 12:26 by hanpeng972
[基金申请] 咱们一起用铁证分析2026国家社科基金中标与否 +7 启萌科技 2026-08-12 22/1100 2026-08-14 23:45 by Noways
[基金申请] 是这周出结果还是下周出结果? +4 yuleib84 2026-08-11 4/200 2026-08-14 23:05 by lfy8008
[基金申请] 奇怪,两个人的filecode固定段从头到尾一模一样 +8 布布和一二 2026-08-10 11/550 2026-08-14 14:58 by Equinoxhua
[硕博家园] 请教兼职经验 +3 是阿文鸭 2026-08-09 3/150 2026-08-14 12:07 by HER12025
[基金申请] FileCode能看出啥? +10 要乐观耀哥 2026-08-10 32/1600 2026-08-14 09:37 by 要乐观耀哥
[文学芳草园] 阿姨 +4 汪汪锅 2026-08-09 4/200 2026-08-13 19:43 by arzu_hma
[基金申请] 重要来源:本周末出结果 +10 瞬息宇宙 2026-08-12 10/500 2026-08-13 15:46 by likettle
[基金申请] 不应该看fileCode +7 且听虎啸 2026-08-12 9/450 2026-08-13 14:27 by flydreamws
[基金申请] Filecode 又变了,巨变 +3 WH3796 2026-08-12 4/200 2026-08-13 14:13 by 小木虫6752397
[基金申请] 分享一下我之前已中青C的计划书的filecode +4 布布和一二 2026-08-11 5/250 2026-08-13 12:56 by cratir
[基金申请] 2019年青年基金涵评意见,大家看看几个A,几个B? +11 Tide man 2026-08-11 11/550 2026-08-13 07:35 by 撸猫猫
[基金申请] 综述论文作为代表作会不会影响评审专家的印象分? +11 yufeiwaner 2026-08-09 13/650 2026-08-12 08:17 by yufeiwaner
[基金申请] 为什么网上很多人说本周 12号出结果 +6 瞬息宇宙 2026-08-10 7/350 2026-08-11 19:25 by Tide man
[基金申请] 什么时候出结果,有咨询渠道??? +3 Tide man 2026-08-11 3/150 2026-08-11 17:54 by kudofaye
[基金申请] 国自然结果 +4 Vierhys 2026-08-10 8/400 2026-08-10 15:06 by Vierhys
信息提示
请填处理意见