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((2R)-1-methylpyrrolidin-2-yl)methanol → (1R/S,2R)-2-Hydroxymethyl-1-(isoxazol-3-ylcarbamoylmethyl)-1-methyl-pyrrolidinium bromide

HRID 1690639
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HRID 1690639 반응식
[Br:1][CH2:2][C:3]([NH:5][C:6]1[CH:10]=[CH:9][O:8][N:7]=1)=[O:4].[CH3:11][N:12]1[CH2:16][CH2:15][CH2:14][C@@H:13]1[CH2:17][OH:18]>C(#N)C>[Br-:1].[OH:18][CH2:17][C@H:13]1[CH2:14][CH2:15][CH2:16][N+:12]1([CH2:2][C:3](=[O:4])[NH:5][C:6]1[CH:10]=[CH:9][O:8][N:7]=1)[CH3:11]
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참가 물질

4

반응물 2

HCID 11007868((2R)-1-methylpyrrolidin-2-yl)methanolHCID 133629192-bromo-N-(isoxazol-3-yl)acetamide2회

생성물 1

HCID 131729615(1R/S,2R)-2-Hydroxymethyl-1-(isoxazol-3-ylcarbamoylmethyl)-1-methyl-pyrrolidinium bromide

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

To a solution of 2-bromo-N-isoxazol-3-yl-acetamide (Intermediate A) (3.9 g, 191 mmol) in acetonitrile (95 ml) is added ((R)-1-methyl-pyrrolidin-2-yl)-methanol (2.2 g, 191 mmol) in acetonitrile (5 ml). The reaction mixture is stirred at room temperature for 3 hours and then the solvent is removed in vacuo. The resulting oil is taken up in acetonitrile and ethyl acetate is then added. The resulting cloudy solution is stirred at room temperature for 30 minutes. There after, the supernatant is decanted off and the solid is dried under vacuum over two days to afford the titled compound.

후처리

  1. customthe solvent is removed in vacuo
  2. additionethyl acetate is then added
  3. stirringThe resulting cloudy solution is stirred at room temperature for 30 minutes
  4. customThere after, the supernatant is decanted off
  5. customthe solid is dried under vacuum over two days

출처 및 근거

ORD 기록
ord-3afe382844e44c5daf037742318bd4e8
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08153669B2

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