反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
Ethyl 2-(1,2,3,4-tetrahydro-2,8-dimethylpyrido[4,3-b]indol-5-yl)acetate (0.5 g, 1.75 mmol) was taken in 4 ml aqueous ammonia and microwaved at 120° C. for 5 min using Initiator (Biotage Microwave). The solid product precipitated out after the reaction was filtered through Buchner funnel and washed with 10% sodium bicarbonate (10 ml×2) followed by demineralised water (10 ml×2) wash. Product was vacuum dried and was taken in 5 ml ethanolic HCl, stirred for 15 minutes, concentrated in vacuo to afford 13 mg of 2-(1,2,3,4-tetrahydro-2,8-dimethylpyrido[4,3-b]indol-5-yl)acetamide as HCl salt. 1H NMR (DMSO) 10.2 (bs, 1H), 7.62 (s, 1H), 7.21-7.3 (m, 3H), 6.9 (d, 1H), 4.75 (s, 2H), 4.45-4.51 (m, 1H), 4.21-4.25 (m, 1H), 3.12-3.17 (m, 4H), 2.97 (s, 3H), 2.19 (s, 3H).
WORKUP
后处理
- custommicrowaved at 120° C. for 5 min
- customThe solid product precipitated out after the reaction
- filtrationwas filtered through Buchner funnel
- washwashed with 10% sodium bicarbonate (10 ml×2)
- washwash
- customdried
- concentrationconcentrated in vacuo