Hydrochloric Acid → HCID 86733143、化合物

HRID 267629ノート

反応式

HRID 267629 の反応式
[OH:1][C@H:2]1[CH2:19][CH2:18][C@@:17]2([CH3:20])[C@@H:4]([CH2:5][CH2:6][C@@H:7]3[C@@H:16]2[C:15](=[O:21])[CH2:14][C@@:12]2([CH3:13])[C@H:8]3[CH2:9][CH2:10][C@@H:11]2[C:22]([O:24][CH3:25])=[O:23])[CH2:3]1.[C:26]1([CH3:36])[CH:31]=[CH:30][C:29]([S:32](Cl)(=[O:34])=[O:33])=[CH:28][CH:27]=1.O.Cl>N1C=CC=CC=1>[CH3:25][O:24][C:22]([C@H:11]1[CH2:10][CH2:9][C@H:8]2[C@H:7]3[C@H:16]([C:15](=[O:21])[CH2:14][C@:12]12[CH3:13])[C@:17]1([CH3:20])[C@H:4]([CH2:3][C@@H:2]([O:1][S:32]([C:29]2[CH:30]=[CH:31][C:26]([CH3:36])=[CH:27][CH:28]=2)(=[O:34])=[O:33])[CH2:19][CH2:18]1)[CH2:5][CH2:6]3)=[O:23]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962Water2 回HCID 73974-Toluenesulfonyl chlorideHCID 867331443beta-Hydroxy-17beta-methoxycarbonyl-5alpha-androstan-11-one

生成物 1

HCID 86733143HCID 86733143、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

3β-Hydroxy-17β-methoxycarbonyl-5α-androstan-11-one (4.75 g.) and toluene-p-sulphonyl chloride (5 g.) in pyridine (50 ml.) were allowed to stand at room temperature for four days. Water (10 ml.) was added, the resulting solution was stirred for an hour and was then poured into stirred water (1.1). The mixture was acidified with hydrochloric acid and the product collected, washed well with water and dried over sodium hydroxide in vacuo. Recrystallisation from chloroform/hexane containing a trace of ether afforded pure title compound (3.4 g.) as needles; m.p. 158°-160°; [α]D + 42.5°, (c 1.09).

後処理

  1. additionwas then poured
  2. customthe product collected
  3. washwashed well with water
  4. dry with materialdried over sodium hydroxide in vacuo
  5. customRecrystallisation from chloroform/hexane containing a trace of ether afforded pure title compound (3.4 g.) as needles
  6. custom[α]D + 42.5°, (c 1.09)

出典と根拠

ORDレコード
ord-02f42a44317341cdbe4e137c38d4bdbf
出典データセット
uspto-grants-1976_03
特許番号
US03943124

反応ノート

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