Triphenylphosphine → HCID 23031297、化合物

HRID 1869684ノート

反応式

HRID 1869684 の反応式
[I-:1].[NH:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH2:7][N+](C)(C)C.[C:12]1([P:18]([C:25]2C=CC=CC=2)[C:19]2C=CC=CC=2)C=CC=CC=1>C(#N)C>[I-:1].[NH:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH2:7][P+:18]([CH3:25])([CH3:19])[CH3:12]

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 139751381H-Pyrrole-2-methanaminium, N,N,N-trimethyl-, iodide (1:1)

生成物 1

HCID 23031297HCID 23031297、化合物収率 152.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Subsequently, to a suspension of (pyrrol-2-yl)methyl trimethylammonium iodide (7.59 g, 28.52 mmol) obtained above in acetonitrile (60 ml) was added triphenylphosphine (8.98 g, 34.2 mmol) with stirring, and the resulting mixture was stirred at 80° C. for 6 hours. After cooling, the reaction mixture was concentrated to about one-half of its initial volume, to which was added ethyl acetate (100 ml). The crystals precipitated were collected by filtration, washed with ethyl acetate and dried in vacuo to afford (pyrrol-2-yl)methyl trimethylphosphonium iodide (12.33 g, yield: 92%).

後処理

  1. stirringthe resulting mixture was stirred at 80° C. for 6 hours
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture was concentrated to about one-half of its initial volume
  4. additionto which was added ethyl acetate (100 ml)
  5. customThe crystals precipitated
  6. filtrationwere collected by filtration
  7. washwashed with ethyl acetate
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-2236918cb45241ffac8b2657f451e37c
出典データセット
uspto-grants-2009_12
特許番号
US07638551B2

反応ノート

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