HRID1190563

反应详情

EQUATION

反应方程式

HRID 1190563 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triphosgene (148 mg, 0.500 mmol) was added to a mixture of 185 mg (0.500 mmol) of 2-(8-bromo-4,5-dihydrothiazolo[4,5-d]benzo[b]oxepine-2-ylamino)-2-methylpropan-1-ol and 0.522 ml (3.00 mmol) of diisopropylethylamine in 7.0 ml of methylene chloride. The reaction mixture was stirred for 3 hours and concentrated in vacuum. The residue was partitioned between ethyl acetate and 5% aqueous citric acid. The organic extracts were washed with water, brine, dried over magnesium sulfate and concentrated in vacuum. Yield 194 mg (98%). MS (ESI+): 396.3

WORKUP

后处理

  1. concentrationconcentrated in vacuum
  2. customThe residue was partitioned between ethyl acetate and 5% aqueous citric acid
  3. washThe organic extracts were washed with water, brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuum