Water → (1-Benzylpyrrolidine-2,5-diyl)dimethanol

HRID 1090511노트

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HRID 1090511 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH:18]([C:19](OCC)=[O:20])[CH2:17][CH2:16][CH:15]1[C:24](OCC)=[O:25])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O>O1CCCC1>[CH2:7]([N:14]1[CH:18]([CH2:19][OH:20])[CH2:17][CH2:16][CH:15]1[CH2:24][OH:25])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 286120Diethyl 1-benzylpyrrolidine-2,5-dicarboxylateHCID 21226445Aluminium lithium hydride2회

생성물 1

HCID 11206806(1-Benzylpyrrolidine-2,5-diyl)dimethanol수율 96.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

To a suspension of lithium aluminum hydride 10.25 g) in tetrahydrofuran (550 ml) was added dropwise a solution of 1-benzyl-2,5-bis(ethoxycarbonyl)pyrrolidine (55 g) in tetrahydrofuran (100 ml). The reaction mixture was stirred for 30 minutes at 0° C., allowed to warm to room temperature and then stirred at the same temperature for 1 hour. And then water was added carefully until excess lithium aluminum hydride was decomposed. After the precipitate was filtered off, the filtrate was evaporated under reduced pressure to give crude 1-benzyl-2,5-bis(hydroxymethyl)pyrrolidine (38.52 g).

후처리

  1. temperatureto warm to room temperature
  2. stirringstirred at the same temperature for 1 hour
  3. filtrationAfter the precipitate was filtered off
  4. customthe filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-2710586f2c8c4f3ead85c734e8887fad
출처 데이터셋
uspto-grants-1992_01
특허 번호
US05081237

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