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HRID20429

反应详情

EQUATION

反应方程式

HRID 20429 的结构方程式

REACTANTS

反应物

3
结构：O=C([O-])[O-].[Cs+].[Cs+]
HCID10796

Cesium carbonate

CCs2O3

结构：FC(F)CBr
HCID136186

2-Bromo-1,1-difluoroethane

C2H3BrF2

结构：CC(=O)N[C@@H](Cc1cccc(O)c1)[C@H](O)[C@H]1CO[C@@H](OCC2(C)CCCC2)CN1C(=O)OC(C)(C)C
HCID68562669

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)N[C@@H](Cc1cccc(OCC(F)F)c1)[C@H](O)[C@H]1CO[C@@H](OCC2(C)CCCC2)CN1C(=O)OC(C)(C)C
HCID58972247

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Dissolve (2R,5R)-5-[(1S,2S)-2-acetylamino-1-hydroxy-3-(3-hydroxyphenyl)-propyl]-2-(1-methylcyclopentylmethoxy)-morpholine-4-carboxylic acid tert-butyl ester (204 mg) and 2,2-difluoro-1-bromoethane (0.065 mL) and cesium carbonate (391 mg) in N,N-dimethylformamide (5 mL) and heat to 60° C. for 18 hours. Dilute with ethyl acetate, wash with saturated aqueous sodium chloride, dry and purify (silica gel chromatography, eluting with 1:1 ethyl acetate:dichloromethane), to give the desired compound (223 mg).

WORKUP

后处理

  1. washwash with saturated aqueous sodium chloride
  2. customdry
  3. custompurify
  4. wash(silica gel chromatography, eluting with 1:1 ethyl acetate:dichloromethane)