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HRID539138

反应详情

EQUATION

反应方程式

HRID 539138 的结构方程式

REACTANTS

反应物

3
结构：O=C(O)C(F)(F)F
HCID6422

未命名化合物

结构：CC[SiH](CC)CC
HCID12052

Silane, triethyl-

C6H16Si

结构：CC(C)[C@H]1NC(=O)[C@@H](C)NC(=O)[C@@H](C(C)C)NC(=O)C[C@@H](/C=C/CCSC(c2ccccc2)(c2ccccc2)c2ccccc2)OOC(=O)C[C@@H]1O
HCID86639580

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)[C@H]1NC(=O)[C@@H](C)NC(=O)[C@@H](C(C)C)NC(=O)C[C@@H](/C=C/CCS)OOC(=O)C[C@@H]1O
HCID25152743

未命名化合物

收率 9.1%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

To a solution of 9 (8 mg, 0.011 mmol) in CH2Cl2 (1 mL) was added triethylsilane (7 μL, 0.44 mmol) was added dropwise TFA (0.2 mL, 20% v/v). After stirring for 1.5 h the reaction was concentrated in vacuo and purified by flash column chromatography (eluent 1:0-99:1-98:2-97:3-96.4 CH2Cl2/MeOH) to give the product 10 (0.47 mg, 0.001 mmol, 9%) as a white solid: Rf 0.44 MeOH/CH2Cl2 (1:9); MS (ES+) 584.2 (100%, [M+Na]+).

WORKUP

后处理

  1. concentrationwas concentrated in vacuo
  2. custompurified by flash column chromatography (eluent 1:0-99:1-98:2-97:3-96.4 CH2Cl2/MeOH)