Hydrochloric Acid → HCID 86733143, 화합물

HRID 267629노트

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HRID 267629 반응식
[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]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962Water2회HCID 73974-Toluenesulfonyl chlorideHCID 867331443beta-Hydroxy-17beta-methoxycarbonyl-5alpha-androstan-11-one

생성물 1

HCID 86733143HCID 86733143, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-02f42a44317341cdbe4e137c38d4bdbf
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03943124

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