Hydrochloric Acid → HCID 54071661, 화합물

HRID 1606378노트

반응식

HRID 1606378 반응식
C1(C)C=CC(S(O[C@H:11]2[CH2:30][CH2:29][C@@:28]3([CH3:31])[C@@H:13]([CH2:14][CH2:15][C@@H:16]4[C@@H:27]3[CH2:26][CH2:25][C@@:24]3([CH3:32])[C@H:17]4[CH2:18][CH:19]=[C:20]3[C:21](=[O:23])[CH3:22])[CH2:12]2)(=O)=O)=CC=1.N1C(C)=CC(C)=CC=1C.Cl>>[CH3:22][C:21](=[O:23])[C:20]1[C@:24]2([CH3:32])[C@H:17]([C@H:16]3[C@H:27]([CH2:26][CH2:25]2)[C@:28]2([CH3:31])[C@H:13]([CH2:12][CH:11]=[CH:30][CH2:29]2)[CH2:14][CH2:15]3)[CH2:18][CH:19]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 79532,4,6-TrimethylpyridineHCID 86733309HCID 86733309, 화합물

생성물 1

HCID 54071661HCID 54071661, 화합물수율 86.5%

실험 절차

3β-Toluene-p-sulphonyloxy-5α-pregn-16-en-20-one (6 g.) was added to hot collidine (12 ml.), and the solution was then refluxed for 30 minutes. The solution was allowed to cool and then poured into cold dilute hydrochloric acid. The precipitate was filtered off, washed with water and dissolved in methylene chloride. The solution was dried over sodium sulphate and then filtered through a short column of silica gel (50 g.). The methylene chloride eluate (about 150 ml.) was evaporated to give 5α-pregna-2,16-dien-20-one (3.29 g.) as white crystals, m.p. 143°-145° , [α]D + 110.5° .

후처리

  1. temperaturethe solution was then refluxed for 30 minutes
  2. temperatureto cool
  3. filtrationThe precipitate was filtered off
  4. washwashed with water
  5. dissolutiondissolved in methylene chloride
  6. dry with materialThe solution was dried over sodium sulphate
  7. filtrationfiltered through a short column of silica gel (50 g.)
  8. customThe methylene chloride eluate (about 150 ml.) was evaporated

출처 및 근거

ORD 기록
ord-f59d3f0db3654eb095975deca1a5fcda
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03952031

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