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

HRID 1782753노트

반응식

HRID 1782753 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8008Butyronitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-93a6c17c3c44457788a844ec68ab49dd
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07498460B2

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