HRID510132
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureafter cooling
- concentrationconcentrated on a rotary evaporator
- custom5 g of the crude product (purity 54%) were obtained