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HRID1488445

反应详情

EQUATION

反应方程式

HRID 1488445 的结构方程式

REACTANTS

反应物

1
结构：C[C@]12C=CC(=O)C=C1CC[C@H]1[C@@H]3C[C@@H](O)[C@](O)(C(=O)CO)[C@@]3(C)C[C@H](O)[C@@]12F
HCID31307

Triamcinolone

C21H27FO6

PRODUCTS

生成物

1
结构：C[C@]12CCC(=O)C=C1CC[C@H]1[C@@H]3C[C@@H](O)[C@](O)(C(=O)CO)[C@@]3(C)C[C@H](O)[C@@]12F
HCID228785

(11β,16α)-9-Fluoro-11,16,17,21-tetrahydroxypregn-4-ene-3,20-dione

C21H29FO6

AUXILIARIES

试剂、催化剂与溶剂

3
结构：[Cl-].[Rh].c1ccc(P(c2ccccc2)c2ccccc2)cc1.c1ccc(P(c2ccccc2)c2ccccc2)cc1.c1ccc(P(c2ccccc2)c2ccccc2)cc1
催化剂HCID84599

未命名化合物

结构：CCO
溶剂HCID702

Ethanol

C2H6O

结构：Cc1ccccc1
溶剂HCID1140

Toluene

C7H8

PROCEDURE

实验过程

A suspension of 3.0 g of tris(triphenylphosphine)rhodium chloride in 1000 ml of degassed toluene was hydrogenated for 45 min at room temperature and atmospheric pressure. A solution of 5.0 g of triamcinolone in 500 ml of absolute ethanol was added and the hydrogenation was continued for 48 h. The reaction mixture was evaporated to dryness and suspended in 50 ml of methylene chloride. After filtration the solid phase was repeatedly washed with small portions of methylene chloride and yielded after drying 4.4 g of 9α-fluoro-11β,16α,17α,21-tetrahydroxypregn-4-ene-3,20-dione. Molecular weight 396 (calc. 396.5).

WORKUP

后处理

  1. waitthe hydrogenation was continued for 48 h
  2. customThe reaction mixture was evaporated to dryness
  3. filtrationAfter filtration the solid phase
  4. washwas repeatedly washed with small portions of methylene chloride
  5. customyielded
  6. dry with materialafter drying 4.4 g of 9α-fluoro-11β,16α,17α,21-tetrahydroxypregn-4-ene-3,20-dione