HRID1095692

反应详情

EQUATION

反应方程式

HRID 1095692 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To tert-butyl 2-methoxy-6-((trimethylsilyl)ethynyl)phenylcarbamate (4.21 g, 13.2 mmol) in MeOH (30 mL) was added K2CO3 (9.11 g, 65.9 mmol). The reaction was stirred for 30 minutes, then filtered and washed with DCM (50 mL). The combined organic layers were concentrated and diluted with DCM (20 mL), filtered, washed a second time with DCM (50 mL), then concentrated. The residue was purified by flash chromatography through a pad of silica gel with 10:1 Hexane/EtOAc (500 mL), affording the desired product (62%).

WORKUP

后处理

  1. filtrationfiltered
  2. washwashed with DCM (50 mL)
  3. concentrationThe combined organic layers were concentrated
  4. additiondiluted with DCM (20 mL)
  5. filtrationfiltered
  6. washwashed a second time with DCM (50 mL)
  7. concentrationconcentrated
  8. customThe residue was purified by flash chromatography through a pad of silica gel with 10:1 Hexane/EtOAc (500 mL)