HRID627759

反应详情

EQUATION

反应方程式

HRID 627759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

To a reaction mixture of tert-butyl ((4aR,11bR)-10-(5-(cyclopropylmethoxy)-3-methylpyrazine-2-carboxamido)-3,3,11b-trimethyl-4,4-dioxido-4a,5,6,11b-tetrahydro-3H-benzo[6,7]oxepino[4,5-b][1,4]thiazin-2-yl)carbamate (40 mg, 0.065 mmol) in DMF 1 ml was added K2CO3 (40 mg, 0.29 mmol). It was heated to 85° C. for 3 h. It was cooled to RT, diluted with water, and extracted with EtOAc. The organic phase obtained was concentrated under reduced pressure and the residue was purified by silica gel chromatography eluting with 15% to 25% to 40% EtOAc/MeOH/Et3N in (40% EtOAc in Heptane) to yield 23 mg of desired product. MS m/z: 514.2 [M+H].

WORKUP

后处理

  1. temperatureIt was cooled to RT
  2. extractionextracted with EtOAc
  3. customThe organic phase obtained
  4. concentrationwas concentrated under reduced pressure
  5. customthe residue was purified by silica gel chromatography
  6. washeluting with 15% to 25% to 40% EtOAc/MeOH/Et3N in (40% EtOAc in Heptane)