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HRID1077191

反应详情

EQUATION

反应方程式

HRID 1077191 的结构方程式

REACTANTS

反应物

3
结构：CCOCC
HCID3283

Diethyl Ether

C4H10O

结构：O=C([O-])O.[Na+]
HCID516892

Sodium Bicarbonate

CHNaO3

结构：CC[C@]12CC[C@@H]3C4=C(CC[C@H]3[C@@H]1CCC21OCCO1)CC(OC)=CC4
HCID10641203

(8'R,9'S,13'S,14'S)-13'-ethyl-3'-methoxyspiro[1,3-dioxolane-2,17'-4,6,7,8,9,11,12,14,15,16-decahydro-1H-cyclopenta[a]phenanthrene]

C22H32O3

PRODUCTS

生成物

1
结构：CC[C@]12CC[C@H]3[C@@H](CCC4=CC(=O)CC[C@@H]43)[C@@H]1CCC2=O
HCID10379264

(+)-13-Ethylgon-4-ene-3,17-dione

C19H26O2

收率 12%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CC(=O)O
溶剂HCID176

Acetic Acid

C2H4O2

结构：O
溶剂HCID962

Water

H2O

PROCEDURE

实验过程

Heat 13β-ethyl-3-methoxy-17,17-ethylenedioxy-gona-2,5(10)-diene (0.1 g.) in glacial acetic acid (2.5 cc.) and water (1 cc.) on a steam bath for 20 minutes, bring finally to boiling and allow to cool. Add aqueous sodium bicarbonate to neutralize the solution and ether extract the product. Wash, dry and evaporate the ether extracts to furnish a residue (0.065 g.); crystallize from a mixture of acetone and light petroleum to obtain the title compound (0.01 g.), m.p. 154°-5°; ultraviolet absorption peak at 239 mμ (ε15,000); infrared absorption peaks at 5.75, 5.96 μ.

WORKUP

后处理

  1. temperatureto cool
  2. extractionextract the product
  3. washWash
  4. customdry
  5. customevaporate the ether
  6. customto furnish a residue (0.065 g.)
  7. customcrystallize from a mixture of acetone and light petroleum