HRID382341

反应详情

EQUATION

反应方程式

HRID 382341 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

cis-4-Benzyloxycarbonylamino-2-methyl-2,3,4,6,7,8-hexahydro-cyclopenta[g]quinoline-1-carboxylic acid ethyl ester (Example 2) (500 mg), 10% palladium on carbon (150 mg), and a mixture of ethanol-cyclohexene (1:1, 50 mL) was heated at reflux for 2 h. The reaction mixture was cooled to room temperature, filtered through Celite®, and concentrated in vacuo. Purification by silica gel chromatography using 5% methanol/ethyl acetate afforded the title compound (350 mg). MS m/z 258 (M+-16); 1H NMR (CDCl3) δ1.1 (d, 3H), 1.3 (t, 3H), 2.1 (m, 2H), 2.4 (m, 1H), 4.2 (m, 2H), 4.5 (m, 1H), 3.8 (dd, 1H), 7.2 (s, 2H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 2 h
  3. filtrationfiltered through Celite®
  4. concentrationconcentrated in vacuo
  5. customPurification by silica gel chromatography