Triphenylphosphine → HCID 21274172、化合物

HRID 1383237ノート

反応式

HRID 1383237 の反応式
[O:1]([C:8]1[CH:9]=[C:10]([CH2:14][CH2:15][CH2:16][Br:17])[CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:18]1([P:24]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>C(#N)C>[Br-:17].[O:1]([C:8]1[CH:9]=[C:10]([CH2:14][CH2:15][CH2:16][P+:24]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 137698271-(3-Bromopropyl)-3-phenoxybenzene

生成物 1

HCID 21274172HCID 21274172、化合物収率 75.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Under nitrogen a mixture of 2.9 grams (0.01 mole) of 3-(3-phenoxyphenyl)propyl bromide and 2.9 grams (0.01 mole) of triphenylphosphine in 25 mL of acetonitrile was heated at reflux overnight. The solvent was evaporated under reduced pressure. Toluene was added to the residue, and this mixture was heated at reflux for 90 minutes during which a solid formed. Filtration yielded 4.2 grams of 3-(3-phenoxyphenyl)propyltriphenylphosphonium bromide, m.p. 198°-200° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. customThe solvent was evaporated under reduced pressure
  4. additionToluene was added to the residue
  5. temperaturethis mixture was heated
  6. temperatureat reflux for 90 minutes during which a solid
  7. customformed
  8. filtrationFiltration

出典と根拠

ORDレコード
ord-254420196a3449c482dbc9a9616c38ca
出典データセット
uspto-grants-1989_02
特許番号
US04808762

反応ノート

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