huagongshe.com
HRID863329

反应详情

EQUATION

反应方程式

HRID 863329 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：[O]=[Cr](=[O])([O-])[O][Cr](=[O])(=[O])[O-].c1cc[nH+]cc1.c1cc[nH+]cc1
HCID2724130

Chromic acid (H2Cr2O7), compd. with pyridine (1:2)

C10H12Cr2N2O7

2 次

结构：CC=CC[C@H](C[C@@H]1OC(C)(C)N(C(=O)OC(C)(C)C)[C@H]1CC(C)(C)CCO)C(=O)NCCCC
HCID86752118

未命名化合物

PRODUCTS

生成物

1
结构：CC=CC[C@H](C[C@@H]1OC(C)(C)N(C(=O)OC(C)(C)C)[C@H]1CC(C)(C)CC(=O)O)C(=O)NCCCC
HCID86752117

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

2 次

PROCEDURE

实验过程

A solution of 809 mg of pyridinium dichromate in 2 ml of N,N-dimethylformamide is added dropwise via a cannula to a solution of 290 mg of 3-[N-tert-butoxycarbonyl-4(S)-(4-hydroxy-2,2-dimethylbutyl)-2,2-dimethyl-1,3-oxazolidin-5(S)-yl]-2(R)-but-2-enyl-propionic acid (N-butyl)amide in 2 ml of N,N-dimethylformamide at room temperature under argon. After 23 h, a further 238 mg of pyridinium dichromate are added. After a total of 29 h, the reaction mixture is poured into water, extracted with diethyl ether (3 times), dried (Na2SO4) and concentrated. Purification over silica gel (mobile phase P) gives the title compound: Rf (P)=0.48; FAB-MS: (M+H)+ =497.

WORKUP

后处理

  1. extractionextracted with diethyl ether (3 times)
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated
  4. customPurification over silica gel (mobile phase P)