反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of TFA/CH2Cl2 (3 mL, 1:1, v:v) was added tert-butyl 6-({[3-[(quinolin-4-ylmethyl)amino]thien-2-yl]carbonyl}amino)indoline-1-carboxylate (40 mg, 0.08 mmol) and the resulting mixture was stirred at rt. After 1 h, the solution was neutralized with 3N NaOH and diluted with EtOAc. The aqueous phase was removed and the organic phase was washed with brine, dried over NaSO4, filtered, and concentrated in vacuo to yield N-2,3-dihydro-1H-indol-6-yl-3-[(quinolin-4-ylmethyl)amino]thiophene-2-carboxamide as a yellow solid. MS (ES+): m/z 401 [M+1]. 1H NMR (CDCl3, 400 MHz): δ3.00 (t, J=8.4 Hz, 2H), 3.58 (t, J=8.4 Hz, 2H), 4.99 (d, J=6.4 Hz, 2H), 6.54 (d, J=5.6 Hz, 1H), 6.67 (d, J=8.0 Hz, 1H), 7.03 (d, J=8.0 Hz, 1H), 7.06 (s, 1H), 7.20 (d, J=5.2 Hz, 1H), 7.46 (d, J=4.4 Hz, 1H), 7.62 (t, J=8.0 Hz, 1H), 7.75 (t, J=8.0 Hz, 1H), 8.03 (m, 2H), 8.16 (d, J=8.0 Hz, 1H), 8.85 (d, J=4.4 Hz, 1H).
WORKUP
后处理
- customThe aqueous phase was removed
- washthe organic phase was washed with brine
- dry with materialdried over NaSO4
- filtrationfiltered
- concentrationconcentrated in vacuo