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Water → HCID 68866327、化合物

HRID 543651
ノート
印刷プレビュー

反応式

HRID 543651 の反応式
[CH3:1][C:2]1[CH2:3][C@H:4]2[C@:17]([CH3:20])([CH2:18][CH:19]=1)[C@@H:16]1[C@H:7]([C@H:8]3[C@@:12]([CH2:14][CH2:15]1)([CH3:13])[C@@H:11]([OH:21])[CH2:10][CH2:9]3)[CH2:6][CH2:5]2.O>CC(C)=O>[CH3:1][C:2]1[CH2:3][C@H:4]2[C@:17]([CH3:20])([CH2:18][CH:19]=1)[C@@H:16]1[C@H:7]([C@H:8]3[C@@:12]([CH2:14][CH2:15]1)([CH3:13])[C:11](=[O:21])[CH2:10][CH2:9]3)[CH2:6][CH2:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 962WaterHCID 228579(5alpha,17beta)-3-Methyl-androst-2-en-17-ol

生成物 1

HCID 68866327HCID 68866327、化合物収率 83.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Kiliani's reagent (100 ml) was added slowly to a solution of 3-methyl-5α-androst-2-en-17β-ol (43 g) in acetone (170 ml). When the addition was complete, water was added to give a precipitate, which was filtered off. The product was redissolved in acetone and water was again added. The precipitate was filtered off, washed with water and dried to give 3-methyl-5α-androst-2-en-17-one (35.7 g). A sample was recrystallised from ether-light petroleum (40°-60°) and from ether to give pure material, m.p. 124°-126°; [α]D +141° (c 0.48 in EtOH).

後処理

  1. additionWhen the addition
  2. customto give a precipitate, which
  3. filtrationwas filtered off
  4. dissolutionThe product was redissolved in acetone
  5. additionwater was again added
  6. filtrationThe precipitate was filtered off
  7. washwashed with water
  8. customdried

出典と根拠

ORDレコード
ord-810a03eb1f6a4191be3e963ad3a83fdd
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04447425

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート