1,2-Bis(chloromethyl)benzene → 2-(Chloromethyl)benzyltri-n-butylphosphonium chloride

HRID 2399645ノート

反応式

HRID 2399645 の反応式
[CH2:1]([P:5]([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[Cl:14][CH2:15][C:16]1[C:17]([CH2:22][Cl:23])=[CH:18][CH:19]=[CH:20][CH:21]=1>C1(C)C=CC=CC=1>[Cl-:14].[Cl:23][CH2:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[CH2:15][P+:5]([CH2:6][CH2:7][CH2:8][CH3:9])([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:1][CH2:2][CH2:3][CH3:4]

参加物

4

反応物 2

HCID 119191,2-Bis(chloromethyl)benzeneHCID 13831Tributylphosphine

生成物 1

HCID 676562342-(Chloromethyl)benzyltri-n-butylphosphonium chloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

A mixture of tri-n-butylphosphine (18.9 g, 103.8 mmol) in toluene (50 mL) was added dropwise to a mixture of α,α'-dichloro-o-xylene (7.0 g, 34.6 mmol) in toluene (200 mL) under argon gas. The reaction mixture was allowed to stir for several days at room temperature under argon, at which time TLC examination showed completion of reaction. Toluene was removed under reduced pressure to give an oily residue. The above oily residue was washed with toluene/hexane (50/50 (v/v), 4×100 mL), and then dried to give a colorless oil. 1H NMR (CDCl3) δ 0.89 (t, 9H), 1.43 (m, 12H), 2.52 (m, 6H), 4.41 (d, 2H), 4.88 (s, 2H), 7.33 (m, 2H), 7.45 (m, 1H), 7.52 (m, 1H).

後処理

  1. customcompletion of reaction
  2. customToluene was removed under reduced pressure
  3. customto give an oily residue
  4. washThe above oily residue was washed with toluene/hexane (50/50 (v/v), 4×100 mL)
  5. customdried
  6. customto give a colorless oil

出典と根拠

ORDレコード
ord-f2a7d95f680842c6892208dfba32a576
出典データセット
uspto-grants-1995_09
特許番号
US05451347

反応ノート

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