Triphenylphosphine → HCID 23031297、化合物

HRID 562644ノート

反応式

HRID 562644 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-4a082b4f34ea4561bfe584cf86571f1c
出典データセット
uspto-grants-2011_11
特許番号
US08067396B2

反応ノート

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