Water → Benzene, 1,1'-(bromomethylene)bis(4chloro-

HRID 602649

反応式

HRID 602649 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)O)=[CH:4][CH:3]=1.B(Br)(Br)[Br:18].O>C(Cl)Cl>[Br:18][CH:8]([C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=1)[C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=1

参加物

5

反応物 3

HCID 962WaterHCID 70334,4'-DichlorobenzhydrolHCID 25134Boron tribromide

生成物 1

HCID 95197Benzene, 1,1'-(bromomethylene)bis(4chloro-

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of 15.14 g (59.3 mmol) of bis(4-chlorophenyl)methanol in 100 mL of methylene chloride was added slowly a solution of 71.2 mL of BBr3 (71.2 mmol, 1M in CH2Cl2). The solution was stirred for at 0° C. for 1 h. Then 60 mL of water was added to quench the reaction and the reaction mixture was poured into 200 mL of methylene chloride. The water layer was extracted with methylene chloride (60 mL×2) and the combined organic layer was dried over Na2SO4 and concentrated to give the title compound; 1NMR (CDCl3) δ 6.24 (s, 1H), 7.36 (d, 4H, J=8.7 Hz), 7.41 (d, 2H, J=8.7 Hz).

後処理

  1. customto quench
  2. customthe reaction
  3. extractionThe water layer was extracted with methylene chloride (60 mL×2)
  4. dry with materialthe combined organic layer was dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-c1e0e25b637a443faee5108660cb8b11
出典データセット
uspto-grants-2011_03
特許番号
US07906503B2

関連ノート

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