反应 #48897

反应方程式

ether

3-methyl-2-((1E,3E)-4-phenylamino-buta-1,3-dienyl)-5-sulfo-1,3-bis-(3-sulfo-propyl)-3H-indolium disodium salt

3-(3-Carboxypropyl)-2,3-dimethyl-5-sulfonato-1-(3-sulfopropyl)-3H-indolium sodium salt

pyridine

→

2-{(1E,3E)-5-[3-(3-carboxy-propyl)-3-methyl-5-sulfo-1-(3-sulfo-propyl)-1,3-dihydro-indole-(2E)-ylidene]-penta-1,3-dienyl}-3-methyl-5-sulfo-1,3-bis-(3-sulfo-propyl)-3 H-indolium tetrasodium salt

溶剂

acetic acid

acetic anhydride

反应条件

后处理

1. 1
   温度under reflux for 15 min
2. 2
   workup.ADDITIONThe obtained precipitate (mixture of the diastereomers
3. 3
   萃取and OB-5.5b) was extracted by suction
4. 4
   洗涤washed with ether
5. 5
   其他dried

实验过程

642 mg (1 mmol) 3-methyl-2-((1E,3E)-4-phenylamino-buta-1,3-dienyl)-5-sulfo-1,3-bis-(3-sulfo-propyl)-3H-indolium disodium salt and 483 mg (1 mmol) 3-(3-Carboxypropyl)-2,3-dimethyl-5-sulfonato-1-(3-sulfopropyl)-3H-indolium sodium salt were dissolved in a mixture of 10 ml acetic acid and 10 ml acetic anhydride. Five ml pyridine was added. The solution was stirred under reflux for 15 min. Twenty ml ether was added after cooling to room temperature. The obtained precipitate (mixture of the diastereomers OB-5.5a and OB-5.5b) was extracted by suction, washed with ether, and dried.

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