HRID1814386

反应详情

EQUATION

反应方程式

HRID 1814386 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(S)-3-[2-Benzyloxy-4-(4-dimethylamino-butanoylamino)-benzenesulfonylamino]-4,4-diethoxy-butyric acid tert-butyl ester (0.62 g, 1.0 mmol) was shaken with 20% palladium on carbon (0.06 g) in THF-EtOH (1:1) under H2 (50 psi) for 16 h using a Parr apparatus. Mass spectrometry and NMR analysis indicated only starting material to be present. An additional 0.28 g of 20% Pd/C and EtOH (50 mL) were added and allowed to stir for 19.5 h. TLC analysis showed complete consumption of starting material. The reaction mixture was filtered through celite and concentrated to yield (S)-3-[4-(4-dimethylamino-butanoylamino)-2-hydroxy-benzensulfonylamino]-4,4-diethoxy-butyric acid tert-butyl ester (0.44 g, 0.83 mmol, 83%). MS (APCI) m/z 532.4 (M+1).

WORKUP

后处理

  1. customconsumption of starting material
  2. filtrationThe reaction mixture was filtered through celite and
  3. concentrationconcentrated