反応 #1908805

反応方程式

sodium hydrosulfite

( 1 )

17-Allylaminogeldanamycin

HCl

dioxane

→

IPI-504

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他The organic layer was collected
2. 2
   乾燥dried over Na2SO4
3. 3
   ろ過filtered
4. 4
   その他transferred to a round bottom flask
5. 5
   workup.STIRRINGto stir under nitrogen for 30 minutes
6. 6
   その他The yellow solid was purified by recrystallization
7. 7
   その他form MeOH/EtOAc

実験手順

Compound of Formula (1) (0.450 g, 0.768 mmol, 1.0 equiv) is dissolved in dichloromethane (50 mL) and stirred with a 10% aqueous solution of sodium hydrosulfite (50 mL). The solution is stirred for 30 minutes. The organic layer was collected, dried over Na2SO4, filtered and transferred to a round bottom flask. To this solution was added a solution of HCl in dioxane (4 N, 0.211 mL, 1.1 equiv.). The resulting mixture was allowed to stir under nitrogen for 30 minutes. A yellow solid slowly crashed out of solution. The yellow solid was purified by recrystallization form MeOH/EtOAc to yield 0.386 g of the IPI-504 (15).

出典