alpha,alpha'-Dichloro-p-xylene → 4-(Chloromethyl)benzyltri-n-butylphosphonium chloride

HRID 2399647

反応式

HRID 2399647 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[CH:21]=[CH:20][C:19]([CH2:22][Cl:23])=[CH:18][CH:17]=1>C1(C)C=CC=CC=1>[Cl-:14].[Cl:23][CH2:22][C:19]1[CH:20]=[CH:21][C:16]([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])=[CH:17][CH:18]=1

参加物

4

反応物 2

HCID 12171alpha,alpha'-Dichloro-p-xyleneHCID 13831Tributylphosphine

生成物 1

HCID 217074094-(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 (7 g, 34.6 mmol, 1 eq.) in toluene (50 mL) was added dropwise to a mixture of α,α'-dichloro-p-xylene (12.1 g, 69.2 mmol, 2 eq.) in toluene (200 mL) under argon gas. The reaction mixture was allowed to stir for 12 hours at room temperature under argon, after which time the tri-n-butylphosphonium chloride salt had crystallized out of solution. The crystals were filtered and washed several times with toluene and hexanes, then air dried: 1H NMR (CDCl3) δ 0.92 (t, 9H), 1.44 (m, 12H), 2.39 (m, 6H), 4.35-4.40 (d, 2H), 4.56 (s, 2H), 7.36-7.39 (d, 2H), 7.47-7.51 (dd, 2H).

後処理

  1. customafter which time the tri-n-butylphosphonium chloride salt had crystallized out of solution
  2. filtrationThe crystals were filtered
  3. washwashed several times with toluene and hexanes
  4. customair dried

出典と根拠

ORDレコード
ord-b8774090357540af89f039c29c390e75
出典データセット
uspto-grants-1995_09
特許番号
US05451347

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