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

HRID 604546
ノート
印刷プレビュー

反応式

HRID 604546 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

(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%).

後処理

  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

出典と根拠

ORDレコード
ord-306edc649297446a8c868c087c7aeb76
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07910617B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート