HRID510132

反应详情

EQUATION

反应方程式

HRID 510132 的结构方程式

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

4.650 g (5.954 mmol) of the compound from example 62 were dissolved in 12 ml of diiodomethane and admixed with 12.76 ml (95.270 mmol) of isopentyl nitrite. The reaction mixture was heated to 85° C. for 16 h and, after cooling, concentrated on a rotary evaporator. 5 g of the crude product (purity 54%) were obtained. 1.2 g of the residue were by means of preparative HPLC (eluent: acetonitrile/water with 0.05% formic acid, gradient 40:60→95:5). 128 mg of the title compound were obtained (15% of theory).

WORKUP

后处理

  1. temperatureafter cooling
  2. concentrationconcentrated on a rotary evaporator
  3. custom5 g of the crude product (purity 54%) were obtained