1,3-Cyclohexanedione → 1,2,3,9-Tetrahydro-6-(phenylmethoxy)-4H-carbazol-4-one

HRID 4382

반응식

HRID 4382 반응식
[C:1]1(=[O:8])[CH2:6][CH2:5][CH2:4][C:3](=O)[CH2:2]1.Cl.[C:10]1([CH2:16][O:17][C:18]2[CH:23]=[CH:22][C:21]([NH:24]N)=[CH:20][CH:19]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C(O)C.O>[C:10]1([CH2:16][O:17][C:18]2[CH:19]=[C:20]3[C:21](=[CH:22][CH:23]=2)[NH:24][C:3]2[CH2:4][CH2:5][CH2:6][C:1](=[O:8])[C:2]3=2)[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

참가 물질

5

반응물 2

HCID 104341,3-CyclohexanedioneHCID 3016725(4-(Benzyloxy)phenyl)hydrazine monohydrochloride

생성물 1

HCID 201524471,2,3,9-Tetrahydro-6-(phenylmethoxy)-4H-carbazol-4-one수율 38.4%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

1,3-Cyclohexanedione (3.1 g) and the product of Stage (i) (5.6 g) in ethanol (196 ml) and water (39 ml) was stirred at room temperature for 3 h and then heated to reflux for 14 h. The resulting solution was allowed to cool, poured into water (500 ml) and the precipitate filtered and washed with isopropyl acetate and ether to give a solid. Recrystallisation from methanol gave the title compound as a solid (2.5 g) m.p. 235°-237°.

후처리

  1. temperatureheated
  2. temperatureto reflux for 14 h
  3. temperatureto cool
  4. filtrationthe precipitate filtered
  5. washwashed with isopropyl acetate and ether
  6. customto give a solid
  7. customRecrystallisation from methanol

출처 및 근거

ORD 기록
ord-78fc489b6c4b4be39c7bb6d9b5564ba7
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725615

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