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小木虫论坛-学术科研互动平台 » 生物医药区 » 新药研发 » 立项调研 » 求助埃索美拉唑钠的旋光值
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caijacky0912

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[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！
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1楼 2012-11-10 09:27:24
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caijacky0912

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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
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3楼2012-11-12 11:55:04
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hardee

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此草有主~

【答案】应助回帖

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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)
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2楼2012-11-10 09:49:31
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hardee

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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°.
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caijacky0912
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4楼2012-11-12 12:44:06
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caijacky0912

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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！
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5楼2012-11-12 21:11:00
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