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

HRID 4382

反応式

HRID 4382 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-78fc489b6c4b4be39c7bb6d9b5564ba7
出典データセット
uspto-grants-1988_02
特許番号
US04725615

関連ノート

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