HRID449839

反应详情

EQUATION

反应方程式

HRID 449839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of (S)-isopropyl 4-((4-chloro-3-methoxypyridin-2-yl)methyl)-7-cyano-1,2,3,4-tetrahydrocyclopenta[b]indol-2-ylcarbamate (12.53 g, 28.55 mmol) and 10% palladium on carbon (1.00 g) in methanol (150 mL) is hydrogenated at 50 psi at room temperature overnight. A fresh batch of 10% palladium on carbon (1.2 g) is slurried in water (˜2 mL) and added to the reaction mixture, which is hydrogenated (50 psi) at room temperature overnight. The catalyst is filtered off and the solution is concentrated under reduced pressure to obtain a pale yellow solid. The solid is triturated with ether twice and dried under high vacuum to afford a yellow solid (10.80 g, 94%). LC-ES/MS m/z 405.2 [M+H]+

WORKUP

后处理

  1. additionadded to the reaction mixture, which
  2. customat room temperature
  3. customovernight
  4. filtrationThe catalyst is filtered off
  5. concentrationthe solution is concentrated under reduced pressure
  6. customto obtain a pale yellow solid
  7. customThe solid is triturated with ether twice
  8. customdried under high vacuum