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Water → alpha-Fluoro-3-phenoxybenzyl alpha-isopropyl-4-chlorophenylacetate

HRID 894337
ノート
印刷プレビュー

反応式

HRID 894337 の反応式
[CH:1]([CH:4]([C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)[C:5]([O-:7])=[O:6])([CH3:3])[CH3:2].[K+].[F:16][CH:17](Br)[C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([O:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:19]=1.O>CN(C)C=O>[CH:1]([CH:4]([C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)[C:5]([O:7][CH:17]([F:16])[C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([O:24][C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:19]=1)=[O:6])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 13194583alpha-Fluoro-3-phenoxybenzylbromideHCID 23685460Potassium alpha-isopropyl-4-chlorophenylacetate

生成物 1

HCID 20507332alpha-Fluoro-3-phenoxybenzyl alpha-isopropyl-4-chlorophenylacetate収率 41.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of potassium α-isopropyl-4-chlorophenylacetate (0.91 g) and α-fluoro-3-phenoxy benzyl bromide (1.06 g) in dimethylformamide (10 ml) was stirred at ambient temperature over a period of 2 hours. The reaction mixture was poured into water and the aqueous solution was extracted with diethyl ether. The ether extract was washed with aqueous sodium carbonate solution and was then dried over anhydrous sodium sulfate. The ether was removed by distillation under reduced pressure and the residue chromatographed over silica gel to give α-fluoro-3-phenoxybenzyl α-isopropyl-4-chlorophenylacetate (0.62 g; 37%) as a colourless oil. The product was characterised by pmr spectroscopy. Chemical shift δppm (solvent CDCl3): 0.69(3H, d, J=6Hz, CH3); 1.05(3H, d of d, J=6Hz and J=2Hz, CH3); 2.34(1H, m, --CH(CH3)2); 3.29 (1H, d, J=10Hz, CH); 7.22(1H, d of d, J=56Hz and J= 2Hz, CHF) and c. 7.24(13H, m, aromatic protons).

後処理

  1. extractionthe aqueous solution was extracted with diethyl ether
  2. extractionThe ether extract
  3. washwas washed with aqueous sodium carbonate solution
  4. dry with materialwas then dried over anhydrous sodium sulfate
  5. customThe ether was removed by distillation under reduced pressure
  6. customthe residue chromatographed over silica gel

出典と根拠

ORDレコード
ord-6fe6199aa5a045ad9efd3530f7f17c09
出典データセット
uspto-grants-1981_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04283414

反応ノート

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