反応 #48897

反応方程式

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

溶媒

acetic acid

acetic anhydride

反応条件

後処理

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

実験手順

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.

出典