HRID54427

反应详情

EQUATION

反应方程式

HRID 54427 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Methyl-4-(3-nitrophenyl) -5-oxo-1,4,5, 6,7,8-hexa-hydro-3-quinolinecarboxylic acid. To a suspension of 2-cyanoethyl 2-methyl-4-(3-nitrophenyl)-5-oxo-1,4,5,6,7,8-hexahydro-3-quinolinecarboxylate (0.47 g) in ethylene glycol dimethyl ether (2 mL) was added 1N sodium hydroxide (4 mL). The mixture was stirred for 20 h, during which time all of the solid went into solution. The mixture was diluted with water, washed with ethyl acetate, and acidified by addition of concentrated hydrochloric acid. The resulting precipitate was collected by vacuum filtration and dried to give the acid as a yellow solid (0.31 g); mp 253°-255° C.; MS: 328 (M); NMR: 1.63-2.00 (m,2, CH2), 2.20 (m,2, CH2), 2.31 (s,3, CH3), 2.49 (m,2, CH2), 5.01 (s,1, CH), 7.49-7.61 (m,2, Ar), 7.97 (m,2, Ar), 9.24 (s, 1, NH). Analysis for C17H16N2O5 : Calculated: C, 62.19; H, 4.91; N, 8.53; Found.: C, 62.16; H, 5.02; N, 8.33.

WORKUP

后处理

  1. washwashed with ethyl acetate
  2. additionacidified by addition of concentrated hydrochloric acid
  3. filtrationThe resulting precipitate was collected by vacuum filtration
  4. customdried