huagongshe.com
HRID1160256

反应详情

EQUATION

反应方程式

HRID 1160256 的结构方程式

REACTANTS

反应物

3
结构：c1c[nH]cn1
HCID795

Imidazole

C3H4N2

结构：CC(C)[Si](Cl)(C(C)C)C(C)C
HCID139400

Triisopropylsilyl chloride

C9H21ClSi

结构：O=C1[C@H](Cc2c(Cl)cc(OCc3ccccc3)cc2Cl)CCN1[C@H]1CC[C@H](O)CC1
HCID178516684

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)[Si](O[C@H]1CC[C@H](N2CC[C@@H](Cc3c(Cl)cc(OCc4ccccc4)cc3Cl)C2=O)CC1)(C(C)C)C(C)C
HCID178460990

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

PROCEDURE

实验过程

Mix (R)-3-(4-Benzyloxy-2,6-dichloro-benzyl)-trans-1-(4-hydroxy-cyclohexyl)-pyrrolidin-2-one (Preparation 16) (1.37 g, 3.07 mmol) and imidazole (0.527 g, 68.08 mmol) in 10 ml of dry DMF. Add triisopropylsilylchloride (0.81 ml, 3.07 mmol) dropwise and stir at room temperature for 5 hours. Quench with 1N HCl and extract with ethyl acetate. Wash the extract with NaHCO3 and brine. Dry over magnesium sulfate, filter, and concentrate. After flash column chromatography, receive 1.83 g (99%) of the title compound: Mass spectrum (apci) m/z=604 (M+H).

WORKUP

后处理

  1. customQuench with 1N HCl
  2. extractionextract with ethyl acetate
  3. washWash the
  4. extractionextract with NaHCO3 and brine
  5. dry with materialDry over magnesium sulfate
  6. filtrationfilter
  7. concentrationconcentrate