Acetone → 2-(Benzyloxy)-1-chloro-3-fluorobenzene

HRID 39015ノート

反応式

HRID 39015 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[OH:9].C([O-])([O-])=O.[K+].[K+].[CH3:16][C:17]([CH3:19])=O>>[CH2:16]([O:9][C:3]1[C:4]([F:8])=[CH:5][CH:6]=[CH:7][C:2]=1[Cl:1])[C:17]1[CH:19]=[CH:4][CH:3]=[CH:2][CH:7]=1

参加物

4

反応物 3

HCID 180AcetoneHCID 11430Potassium CarbonateHCID 27737102-Chloro-6-fluorophenol

生成物 1

HCID 532169822-(Benzyloxy)-1-chloro-3-fluorobenzene

反応条件

温度
65 °C

実験手順

A mixture of 2-chloro-6-fluorophenol (25 g, 170 mmol), acetone (200 ml), K2CO3 (47.08 g, 340 mmol) and bensylbromide (22.31 ml, 187 mmol) was heated at 65° C. for 16 h. The solution was filtered and evaporated. Water (100 ml) was added, and the solution was extracted with EtOAc. The combined organic phases were dried (Na2SO4) and evaporated to dryness to give the title compound (32.3 g). MS m/z (rel. intensity, 70 eV) 236 (M+, 2), 117 (4), 92 (8), 91 (bp), 65 (13).

後処理

  1. filtrationThe solution was filtered
  2. customevaporated
  3. additionWater (100 ml) was added
  4. extractionthe solution was extracted with EtOAc
  5. dry with materialThe combined organic phases were dried (Na2SO4)
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-38288b2fe72543d2874ba82dd88f7891
出典データセット
uspto-grants-2013_09
特許番号
US08524766B2

反応ノート

読み込み中…