Water → 1-(3-Methoxyphenyl)-2-(1-methyl-2-pyrrolidinyl)ethanone

HRID 2049653

반응식

HRID 2049653 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[CH:10]=[C:11]([C:15](=[O:23])[CH:16]=[C:17]2[CH2:21][CH2:20][CH2:19][N:18]2[CH3:22])[CH:12]=[CH:13][CH:14]=1.O.C(OCC)C>O1CCCC1>[CH3:7][O:8][C:9]1[CH:10]=[C:11]([C:15](=[O:23])[CH2:16][CH:17]2[CH2:21][CH2:20][CH2:19][N:18]2[CH3:22])[CH:12]=[CH:13][CH:14]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 3283Diethyl EtherHCID 21226445Aluminium lithium hydrideHCID 571537451-(3-Methoxyphenyl)-2-(1-methyl-2-pyrrolidinyliden)ethanone

생성물 1

HCID 203441421-(3-Methoxyphenyl)-2-(1-methyl-2-pyrrolidinyl)ethanone

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

11.8 g of lithium aluminum hydride are added portionwise at 0° with stirring to 144.8 g of 1-(3-methoxyphenyl)-2-(1-methyl-2-pyrrolidinyliden)ethanone dissolved in 1.4 liters of tetrahydrofuran. 30 minutes after completion of the addition, 300 ml of water are cautiously added dropwise, with cooling; then 800 ml of diethyl ether are added, and the organic phase is collected. The organic phase is dried over sodium sulfate, the solvent is removed by evaporation, and the oily residue is distilled under a vacuum to obtain 127 g (87% of theory) of the title compound:

후처리

  1. additionare cautiously added dropwise
  2. temperaturewith cooling
  3. customthe organic phase is collected
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customthe solvent is removed by evaporation
  6. distillationthe oily residue is distilled under a vacuum

출처 및 근거

ORD 기록
ord-7820fc9e1cab48449fbfec1eb3cd7a56
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04198424

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