HRID268711

反应详情

EQUATION

反应方程式

HRID 268711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of N-t-butoxycarbonyl-5-methoxycarbonylisoindoline (D12) (2.11 g) in MeOH (10 ml) was treated with 1M NaOH and heated at 60° C. for 1 h. The mixture was cooled to rt and the MeOH evaporated. The aqueous was washed with diethyl ether (2×20 ml), then acidified with 5% citric acid solution and extracted with diethyl ether (2×20 ml). The combined extracts were washed with water (2×20 ml), brine (20 ml), dried (MgSO4) and evaporated to give the title compound (D13) (1.47 g). MS electrospray (+ion) 264 (MH+). 1H NMR δ (CDCl3): 8.02 (2H, m), 7.35 (1H, m), 4.75 (2H, s), 4.71 (2H, s), 1.53 (9H, s).

WORKUP

后处理

  1. temperatureThe mixture was cooled to rt
  2. customthe MeOH evaporated
  3. washThe aqueous was washed with diethyl ether (2×20 ml)
  4. extractionextracted with diethyl ether (2×20 ml)
  5. washThe combined extracts were washed with water (2×20 ml), brine (20 ml)
  6. dry with materialdried (MgSO4)
  7. customevaporated