Water → HCID 20344133, 화합물

HRID 2049654노트

반응식

HRID 2049654 반응식
[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

참가 물질

6

반응물 4

HCID 962WaterHCID 322000HCID 322000, 화합물HCID 4432340PicrateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 20344133HCID 20344133, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-f78419e6e29d4ee18fd6c875f910ddb8
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04198424

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