Benzene, 1,3-bis(chloromethyl)- → 3-(Chloromethyl)benzyltri-n-butylphosphonium chloride

HRID 2399646

反応式

HRID 2399646 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][CH:19]=[C:18]([CH2:22][Cl:23])[CH:17]=1>C1(C)C=CC=CC=1>[Cl-:14].[Cl:23][CH2:22][C:18]1[CH:17]=[C:16]([CH:21]=[CH:20][CH:19]=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 12275Benzene, 1,3-bis(chloromethyl)-HCID 13831Tributylphosphine

生成物 1

HCID 676565363-(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-m-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, after which time the tri-n-butylphosphonium chloride salt had crystallized out of solution and TLC examination showed completion of reaction. The white crystals were filtered and washed several times with toluene and hexanes, and then dried. 1H NMR (CDCl3) δ 0.93 (t, 9H), 1.45 (m, 12H), 2.41 (m, 6H), 4.40 (d, 2H), 4.57 (s, 2H), 7.36 (m, 2H), 7.42 (d, 2H).

後処理

  1. customafter which time the tri-n-butylphosphonium chloride salt had crystallized out of solution and TLC examination
  2. customcompletion of reaction
  3. filtrationThe white crystals were filtered
  4. washwashed several times with toluene and hexanes
  5. customdried

出典と根拠

ORDレコード
ord-ededb267cad641e9a7f04d2a0d38f761
出典データセット
uspto-grants-1995_09
特許番号
US05451347

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