Potassium Carbonate → 3-[4-(1,1'-Biphenyl-4-ylmethoxy)phenyl]-1-propanol

HRID 1782753ノート

反応式

HRID 1782753 の反応式
[C:1]1([C:7]2[CH:14]=[CH:13][C:10]([CH2:11]Br)=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH:15][C:16]1[CH:21]=[CH:20][C:19]([CH:22](O)[CH2:23][CH3:24])=[CH:18][CH:17]=1.C(=O)([O-])[O-:27].[K+].[K+]>C(#N)CCC>[C:7]1([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH:14]=[CH:13][C:10]([CH2:11][O:15][C:16]2[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][CH2:24][OH:27])=[CH:18][CH:17]=2)=[CH:9][CH:8]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 2577161,1'-Biphenyl, 4-(bromomethyl)-HCID 130555574-(1-Hydroxypropyl)Phenol

生成物 1

HCID 575890363-[4-(1,1'-Biphenyl-4-ylmethoxy)phenyl]-1-propanol

試薬・触媒・溶媒 1

HCID 8008Butyronitrile溶媒

実験手順

12.8 g (41.4 mmol) of 4-phenylbenzyl bromide, 6.94 g (45.6 mmol) of 4-hydroxy-phenylpropanol and 6.87 g (49.7 mmol) of potassium carbonate are stirred in 50 ml of butyronitrile at 120° C. for 6 hours. Cooling to room temperature is followed by removal of the inorganic salts by filtration with suction and concentration in vacuo. The crude product is purified by chromatography on silica gel 60 (mobile phase gradient cyclohexane-->cyclohexane/ethyl acetate 60:40). 4.90 g (37% of theory) of product are obtained.

後処理

  1. customis followed by removal of the inorganic salts by filtration with suction and concentration in vacuo
  2. customThe crude product is purified by chromatography on silica gel 60 (mobile phase gradient cyclohexane-->cyclohexane/ethyl acetate 60:40)
  3. custom4.90 g (37% of theory) of product are obtained

出典と根拠

ORDレコード
ord-93a6c17c3c44457788a844ec68ab49dd
出典データセット
uspto-grants-2009_03
特許番号
US07498460B2

反応ノート

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