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HRID1650116

反应详情

EQUATION

反应方程式

HRID 1650116 的结构方程式

REACTANTS

反应物

3
结构：CCC[CH2][Sn+]([CH2]CCC)[CH2]CCC.C[O-]
HCID11964040

未命名化合物

结构：CC[C@]12CC[C@@H]3c4ccc(OC)cc4CC[C@H]3[C@@H]1CC=C2OC(C)=O
HCID14257187

未命名化合物

结构：C=CCCOC(=O)[O-]
HCID23349072

未命名化合物

PRODUCTS

生成物

1
结构：CC[C@]12CC[C@@H]3c4ccc(OC)cc4CC[C@H]3[C@@H]1C=CC2=O
HCID14257189

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

3
结构：CC(=O)[O-].CC(=O)[O-].[Pd+2]
催化剂HCID167845

Diacetatopalladium

C4H6O4Pd

结构：O
溶剂HCID962

Water

H2O

结构：CC#N
溶剂HCID6342

Acetonitrile

C2H3N

PROCEDURE

实验过程

3.4 g of 17-acetoxy-3-methoxy-18-methyl-1,3,5(10),16-estratetraene is refluxed for 1.5 hours in 50 ml of acetonitrile with 2.3 ml of allylmethylcarbonate, 220 mg of palladium acetate and 580 microliters of tributyltin methoxide. The reaction mix is then diluted with water, extracted with dichloromethane and concentrated under vacuum. After chromatographic purification, 2.1 g of 3-methoxy-18-methyl-1,3,5(10),15-estratetraen-17-one with a melting point of 158°-160° C. is obtained.

WORKUP

后处理

  1. additionThe reaction mix
  2. extractionextracted with dichloromethane
  3. concentrationconcentrated under vacuum
  4. customAfter chromatographic purification, 2.1 g of 3-methoxy-18-methyl-1,3,5(10),15-estratetraen-17-one with a melting point of 158°-160° C.
  5. customis obtained