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Triphenylphosphine → (1-Methylpyrrol-2-yl)methyltriphenylphosphonium iodide

HRID 604546
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HRID 604546 반응식
[I-:1].[CH3:2][N:3]1[CH:7]=[CH:6][CH:5]=[C:4]1[CH2:8][N+](C)(C)C.[C:13]1([P:19]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(#N)C>[I-:1].[CH3:2][N:3]1[CH:7]=[CH:6][CH:5]=[C:4]1[CH2:8][P+:19]([C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1
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참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 12346658N,N,N-Trimethyl(1-methyl-1H-pyrrol-2-yl)methanaminium iodide

생성물 1

HCID 23031470(1-Methylpyrrol-2-yl)methyltriphenylphosphonium iodide수율 81%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
80 °C

실험 절차

(1-Methylpyrrol-2-yl)methyltrimethylammonium iodide (55.3 g, 198 mmol) was suspended in acetonitrile (400 mL) and triphenylphosphine (62.2 g, 237 mmol) was added thereto, followed by stirring of the mixture at 80° C. for 10 hours. After cooling, the mixture was concentrated to about 1/2 under reduced pressure, ethyl acetate (200 mL) was added thereto, and the precipitated crystal was collected by filtration. The crystal was washed with ethyl acetate and dried under reduced pressure to obtain the title compound (77.1 g, yield: 81%).

후처리

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated to about 1/2 under reduced pressure, ethyl acetate (200 mL)
  3. additionwas added
  4. filtrationthe precipitated crystal was collected by filtration
  5. washThe crystal was washed with ethyl acetate
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-306edc649297446a8c868c087c7aeb76
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07910617B2

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