Water → 1,1'-Biphenyl, 4-(bromomethyl)-

HRID 466228

반응식

HRID 466228 반응식
[C:1]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][C:4]([CH2:7]O)=[CH:3][CH:2]=1.P(Br)(Br)[Br:16].C(Cl)Cl.O>CCCCCC.C(OCC)(=O)C>[CH:12]1[CH:13]=[CH:14][C:9]([C:1]2[CH:6]=[CH:5][C:4]([CH2:7][Br:16])=[CH:3][CH:2]=2)=[CH:10][CH:11]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 6344DichloromethaneHCID 19186(1,1'-Biphenyl)-4-methanolHCID 24614Phosphorus tribromide

생성물 1

HCID 2577161,1'-Biphenyl, 4-(bromomethyl)-

시약·촉매·용매 2

HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

실험 절차

A suspension of 4-biphenylmethanol (62.9 g, 340 mmol) in hexane (650 mL) is treated with phosphorus tribromide (16 mL, 171 mmol) dropwise over 10 minutes. After 20 minutes CH2Cl2 (200 mL) is added to dissolve the remaining solid. The solution is then stirred for 1.5 hours and treated with water (200 mL) and then ethyl acetate. The organic layer is washed with water, cold saturated sodium bicarbonate and water, dried over sodium sulfate and evaporated to dryness to yield 4-biphenylmethyl bromide, m.p. 79°-80° C.

후처리

  1. dissolutionto dissolve the remaining solid
  2. washThe organic layer is washed with water, cold saturated sodium bicarbonate and water
  3. dry with materialdried over sodium sulfate
  4. customevaporated to dryness

출처 및 근거

ORD 기록
ord-b5b875fe91a04f30b1bbf095aa6869d6
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155100

연결된 노트

불러오는 중…