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
- 50 °C
PROCEDURE
实验过程
Tetrabutylammonium flouride (1M in THF, 5 ml, 5 mmol) was added to 3-[2-(trimethylsilyl)ethoxycarbonylamino]-4-ethyl-9-isopropyl-9H-pyrido[3,4-b]indole (Method 4; 80 mg, 0.2 mmol) and the mixture was heated to 50° C. for 1 hour. The mixture was concentrated in vacuo and the residue was dissolved in DCM and washed with water. The organic phase was separated, dried and evaporated in vacuo. The crude product was purified by flash eluting over a gradient of 0-2.5% MeOH in DCM. The product was obtained as a light brown solid (34 mg) after evaporation of the appropriate fractions. NMR (300 MHz, CDCl3) 8.40 (s, 1H), 8.16 (d, 1H), 7.48 (m, 2H), 7.18 (t, 1H), 4.91 (m, 1H), 3.13 (q, 2H), 1.69 (d, 6H), 1.40 (t, 3H); m/z 255.
WORKUP
后处理
- concentrationThe mixture was concentrated in vacuo
- dissolutionthe residue was dissolved in DCM
- washwashed with water
- customThe organic phase was separated
- customdried
- customevaporated in vacuo
- customThe crude product was purified by flash
- washeluting over a gradient of 0-2.5% MeOH in DCM