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

HRID 602649

반응식

HRID 602649 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c1e0e25b637a443faee5108660cb8b11
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906503B2

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