huagongshe.com
HRID20399

反应详情

EQUATION

反应方程式

HRID 20399 的结构方程式

REACTANTS

反应物

3
结构：CC(=O)OC(C)=O
HCID7918

Acetic anhydride

C4H6O3

结构：CCN(CC)CC
HCID8471

Triethylamine

C6H15N

结构：CC(C)(C)OC(=O)N1CC(c2ccccc2)(c2ccccc2)OC[C@@H]1[C@@H](O)[C@@H](N)Cc1cc(F)cc(F)c1
HCID68561345

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)N[C@@H](Cc1cc(F)cc(F)c1)[C@H](O)[C@H]1COC(c2ccccc2)(c2ccccc2)CN1C(=O)OC(C)(C)C
HCID68561953

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

Dissolve (R)-5-[(1S,2S)-2-amino-3-(3,5-difluorophenyl)-1-hydroxypropyl]-2,2-diphenylmorpholine-4-carboxylic acid tert-butyl ester (0.163 g, 0.31 mmol) in tetrahydrofuran (4 mL). Add triethylamine (0.044 g, 0.44 mmol) and acetic anhydride (0.036 g, 0.35 mmol). Stir 90 minutes and dilute with ethyl acetate (50 mL). Wash with 0.1 N aqueous citric acid, water, and saturated aqueous sodium chloride. Dry (magnesium sulfate), filter and concentrate. Purify on silica gel, eluting with 10:90 to 50:50 ethyl acetate:hexanes to give the title compound.

WORKUP

后处理

  1. washWash with 0.1 N aqueous citric acid, water, and saturated aqueous sodium chloride
  2. dry with materialDry (magnesium sulfate)
  3. filtrationfilter
  4. concentrationconcentrate
  5. customPurify on silica gel
  6. washeluting with 10:90 to 50:50 ethyl acetate