Water → HCID 20344133、化合物

HRID 2049654ノート

反応式

HRID 2049654 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[CH:9]=[C:10]([C:14](=[O:22])[CH:15]=[C:16]2[CH2:20][CH2:19][CH2:18][N:17]2[CH3:21])[CH:11]=[CH:12][CH:13]=1.O.C1(C([O-])=C([N+]([O-])=O)C=C([N+]([O-])=O)C=1)[N+]([O-])=O>O1CCCC1>[CH3:7][C:8]1[CH:9]=[C:10]([C:14](=[O:22])[CH2:15][CH:16]2[CH2:20][CH2:19][CH2:18][N:17]2[CH3:21])[CH:11]=[CH:12][CH:13]=1

参加物

6

反応物 4

HCID 962WaterHCID 322000HCID 322000、化合物HCID 4432340PicrateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 20344133HCID 20344133、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5.8 g of lithium aluminum hydride are added portionwise at 0° to 66 g of 1-(3-methylphenyl)-2-(1-methyl-2-pyrrolidinyliden)ethanone dissolved in 550 ml of tetrahydrofuran. 20 minutes after completion of the addition, water is added dropwise until no evolution of gas is any longer observed. The light-yellow organic phase is decanted from the formed precipitate, the latter is extracted with diethyl ether, the united organic phases are dried over sodium sulfate and concentration to an oil is effected. After distillation under vacuum, 61.7 g (92% of theory) of the title compound (b.p. 116° at 0.01 mm Hg) are obtained. Picrate (from ethanol): m.p. 146° to 149°.

後処理

  1. additionis added dropwise until no evolution of gas
  2. customThe light-yellow organic phase is decanted from the formed precipitate
  3. extractionthe latter is extracted with diethyl ether
  4. dry with materialthe united organic phases are dried over sodium sulfate and concentration to an oil
  5. distillationAfter distillation under vacuum, 61.7 g (92% of theory) of the title compound (b.p. 116° at 0.01 mm Hg)
  6. customare obtained

出典と根拠

ORDレコード
ord-f78419e6e29d4ee18fd6c875f910ddb8
出典データセット
uspto-grants-1980_04
特許番号
US04198424

反応ノート

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