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HRID481246

反应详情

EQUATION

反应方程式

HRID 481246 的结构方程式

REACTANTS

反应物

2
结构：COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
HCID87949

p-Anisyldithiophosphonic anhydride

C14H14O2P2S4

结构：CC(C)(C)OC(=O)[C@@H]1C[C@@H](CCCc2ccccc2)C(=O)N1
HCID86587563

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)[C@@H]1CC(CCCc2ccccc2)C(=S)N1
HCID86587564

未命名化合物

收率 179.8%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：c1ccccc1
溶剂HCID241

Benzene

C6H6

PROCEDURE

实验过程

A mixture of pyroglutamate 8c (245.4 mg, 0.809 mmol) and Lawesson's reagent (164 mg, 0.404 mmol) in 6 mL benzene was stirred at reflux for 17 h, then concentrated. The crude product was purified by flash chromatography (0.5 to 1 to 1.5 to 2% MeOH/CHCl3) to afford 232 mg (90%) of the thiolactam 8d as a 2:1 mixture of diastereomers.

WORKUP

后处理

  1. temperatureat reflux for 17 h
  2. concentrationconcentrated
  3. customThe crude product was purified by flash chromatography (0.5 to 1 to 1.5 to 2% MeOH/CHCl3)