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HRID1838883

反应详情

EQUATION

反应方程式

HRID 1838883 的结构方程式

REACTANTS

反应物

4
结构：Cc1ccc(S(=O)(=O)O)cc1
HCID6101

4-Methylbenzenesulfonic acid

C7H8O3S

结构：C1=COCCC1
HCID8080

3,4-Dihydro-2H-pyran

C5H8O

结构：CCN(CC)CC
HCID8471

Triethylamine

C6H15N

结构：CC(=O)OCCCCC[C@@H]1Cc2cc(O)ccc2[C@@H]2[C@@H]1[C@@H]1CCC(=O)[C@@]1(C)C[C@@H]2F
HCID69935119

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)OCCCCC[C@@H]1Cc2cc(OC3CCCCO3)ccc2[C@@H]2[C@@H]1[C@@H]1CCC(=O)[C@@]1(C)C[C@@H]2F
HCID22941806

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

8.2 g of 7α-(5-acetoxypentyl)-11β-fluoro-3-hydroxyestra-1,3,5(10)-trien-17-one in 86 ml of THF are stirred at RT for 2.5 h with 8.6 ml of 3,4-dihydro-2H-pyran and 820 mg of p-toluenesulphonic acid. 0.5 ml of triethylamine is then added, and the mixture is diluted with ethyl acetate, washed with saturated sodium chloride solution, dried and concentrated in vacuo. After chromatographing the crude product on silica gel using a hexane-ethyl acetate gradient, 7.8 g of 7α-(5-acetoxypentyl)-11β-fluoro-3-(tetrahydropyran-2-yloxy) oestra-1,3,5(10)-trien-17-one are obtained as a foam.

WORKUP

后处理

  1. washwashed with saturated sodium chloride solution
  2. customdried
  3. concentrationconcentrated in vacuo
  4. customare obtained as a foam