HRID471300

反应详情

EQUATION

反应方程式

HRID 471300 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl 3-(3-((4-(2-methylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)methyl)phenethoxy)propanoate (Example 277, step a) was dissolved in DCM (10 mL) and TFA (2 mL) was added. The resulting mixture was stirred for 2 h then evaporated. The residue was azeotroped with toluene and redissolved in MeCN (10 mL). This was applied to a SCX cartridge (50 g, Varian) which had been pre-wetted with MeCN. The cartridge was washed with MeCN (100 mL) and eluted with 880 aqueous ammonia in MeCN (1:4, 100 mL). The eluent was evaporated to afford the subtitled compound. Material used directly in the next step.

WORKUP

后处理

  1. customthen evaporated
  2. customThe residue was azeotroped with toluene
  3. dissolutionredissolved in MeCN (10 mL)
  4. washThe cartridge was washed with MeCN (100 mL)
  5. washeluted with 880 aqueous ammonia in MeCN (1:4, 100 mL)
  6. customThe eluent was evaporated