HRID215750

反应详情

EQUATION

反应方程式

HRID 215750 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A 15 mL flask was charged with 3-amino-4,5,6,7-tetrahydro-benzo[b]thiophene-2-carboxylic acid ethyl ester (synthesized by the route described in Example 5, Step A; 0.50 g, 2.4 mmol), formamide (4.8 mL), and KOtBu (95%; 0.56 g, 4.8 mmol) under N2. After heating at 110° C. for 12 h, the mixture was poured over cold satd. aq. NH4Cl (10 mL). Filtration afforded the desired product (0.31 g). MS: No signal. 1H NMR (400 MHz, d6-DMSO) δ ppm 8.00 (s, 1H), 2.74-2.69 (m, 2H), 2.56-2.51 (m, 2H), 1.92-1.81 (m, 2H), 1.79-1.69 (m, 2H).

WORKUP

后处理

  1. customsynthesized by the route
  2. additionthe mixture was poured over cold satd
  3. filtrationFiltration