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

HRID 487224

反応式

HRID 487224 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b747980d6f6741a5a197a302a8d0fac7
出典データセット
uspto-grants-1994_03
特許番号
US05294632

関連ノート

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