HRID392960

反应详情

EQUATION

反应方程式

HRID 392960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

A 60% dispersion of sodium hydride in mineral oil (50 mg, 1.25 mmol) was added in a single portion to a stirred mixture of compound 6 in DMF (3.5 mL). When the rapid evolution of hydrogen had ceased, the mixture was cooled in an ice-water bath. Diphenylmethyl bromide (297 mg, 1.2 mmol) was added. The mixture was stirred at an oil bath temperature of 55° C. for 30 min. The mixture was cooled and poured into cold water to precipitate a solid. The solid was dried and crystallized from ethyl acetate-hexanes to afford 8 as off white needles. ESI-MS m/e 484 (M+1).

WORKUP

后处理

  1. temperaturethe mixture was cooled in an ice-water bath
  2. temperatureThe mixture was cooled
  3. customto precipitate a solid
  4. customThe solid was dried
  5. customcrystallized from ethyl acetate-hexanes
  6. customto afford 8 as off white needles