Water → 21-Morpholino-5alpha-pregnane-3,11,20-trione

HRID 1576794ノート

反応式

HRID 1576794 の反応式
Br[CH2:2][C:3](=[O:25])[C@@H:4]1[C@:21]2([CH3:22])[C@H:7]([C@H:8]3[C@H:18]([C:19](=[O:23])[CH2:20]2)[C@:16]2([CH3:17])[C@H:11]([CH2:12][C:13](=[O:24])[CH2:14][CH2:15]2)[CH2:10][CH2:9]3)[CH2:6][CH2:5]1.[NH:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1.O>O1CCCC1>[O:29]1[CH2:30][CH2:31][N:26]([CH2:2][C:3](=[O:25])[C@@H:4]2[C@:21]3([CH3:22])[C@H:7]([C@H:8]4[C@H:18]([C:19](=[O:23])[CH2:20]3)[C@:16]3([CH3:17])[C@H:11]([CH2:12][C:13](=[O:24])[CH2:14][CH2:15]3)[CH2:10][CH2:9]4)[CH2:6][CH2:5]2)[CH2:27][CH2:28]1

参加物

5

反応物 3

HCID 962WaterHCID 8083MorpholineHCID 8673347421-Bromo-5alpha-pregnane-3,11,20-trione

生成物 1

HCID 8673403221-Morpholino-5alpha-pregnane-3,11,20-trione

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-c0680a7ade3741f5a799f8210d04c6d7
出典データセット
uspto-grants-1976_09
特許番号
US03983111

反応ノート

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