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Sodium potassium tartrate tetrahydrate → Progesterone Impurity D

HRID 1385618
ノート
印刷プレビュー

反応式

HRID 1385618 の反応式
[C:1]([O:4][C@H:5]([C@@H:7]1[C@:24]2([CH3:25])[C@H:10]([C@H:11]3[C@H:21]([CH2:22][CH2:23]2)[C@:19]2([CH3:20])[C:14]([CH2:15][C@@H:16]([OH:26])[CH2:17][CH2:18]2)=[CH:13][CH2:12]3)[CH2:9][CH2:8]1)[CH3:6])(=[O:3])[CH3:2].O.O.O.O.C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1.CC(=O)CC.O>[C:1]([O:4][C@H:5]([C@@H:7]1[C@:24]2([CH3:25])[C@H:10]([C@H:11]3[C@H:21]([CH2:22][CH2:23]2)[C@:19]2([CH3:20])[C:14](=[CH:15][C:16](=[O:26])[CH2:17][CH2:18]2)[CH2:13][CH2:12]3)[CH2:9][CH2:8]1)[CH3:6])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 2724148Sodium potassium tartrate tetrahydrateHCID 21969303(3beta,20S)-pregn-5-ene-3,20-diol 20-acetate

生成物 1

HCID 57099835Progesterone Impurity D収率 82.2%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 1140Toluene溶媒
HCID 6569
Methyl Ethyl Ketone
溶媒

実験手順

—Aluminium isopropoxide (18.1 g) was added to a solution of (3β,20S)-pregn-5-ene-3,20-diol 20-acetate (21.9 g) in dry toluene (252 ml) and dry 2-butanone (156 ml). The mixture was heated under reflux for 2 h, then cooled, whereupon a solution of potassium sodium tartrate tetrahydrate (91.4 g) in water (90 ml) was added. The mixture was stirred for 30 min. and filtered. The filtrate was poured into brine and the product extracted into ethyl acetate. The combined organic phases were washed with brine, dried over sodium sulfate, and concentrated under reduced pressure. Column chromatography afforded (20S)-20-(acetyloxy)pregn-4-en-3-one (compound 6; 17.9 g).

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 h
  3. additionwas added
  4. filtrationfiltered
  5. additionThe filtrate was poured into brine
  6. extractionthe product extracted into ethyl acetate
  7. washThe combined organic phases were washed with brine
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-5ec231da438b4998a4b701af36a73ae9
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06262282B1

反応ノート

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