huagongshe.com
HRID1576794

反应详情

EQUATION

反应方程式

HRID 1576794 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：C1COCCN1
HCID8083

Morpholine

C4H9NO

结构：C[C@]12CCC(=O)C[C@@H]1CC[C@H]1[C@@H]3CC[C@H](C(=O)CBr)[C@@]3(C)CC(=O)[C@@H]12
HCID86733474

未命名化合物

PRODUCTS

生成物

1
结构：C[C@]12CCC(=O)C[C@@H]1CC[C@H]1[C@@H]3CC[C@H](C(=O)CN4CCOCC4)[C@@]3(C)CC(=O)[C@@H]12
HCID86734032

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

A solution of 21-bromo-5α-pregnane-3,11,20-trione (500 mg) in dry tetrahydrofuran was treated at reflux with morpholine (0.5 ml) for 1/2 hour, and poured into water. The oily precipitate was extracted into ether and the extracts were washed with water, dried (Na2SO4) and evaporated to the crude product which was purified by preparative t.l.c. in ethyl acetate and crystallisation from ether to give the title compound (220 mg). m.p. 159°-164°C [α]D +98° (c=1.1%)

WORKUP

后处理

  1. extractionThe oily precipitate was extracted into ether
  2. washthe extracts were washed with water
  3. dry with materialdried (Na2SO4)
  4. customevaporated to the crude product which
  5. customwas purified by preparative t.l.c
  6. customin ethyl acetate and crystallisation from ether