Hydrochloric Acid → 8-(4-(Trifluoromethoxy)-phenoxy)-1-octanol

HRID 439751

反応式

HRID 439751 の反応式
[F:1][C:2]([F:12])([F:11])[O:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.Br[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][OH:22].C([O-])([O-])=O.[K+].[K+].Cl>CN(C)C=O>[F:1][C:2]([F:11])([F:12])[O:3][C:4]1[CH:5]=[CH:6][C:7]([O:10][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][OH:22])=[CH:8][CH:9]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 70015p-(Trifluoromethoxy)phenolHCID 1626071-Octanol, 8-bromo-

生成物 1

HCID 224079298-(4-(Trifluoromethoxy)-phenoxy)-1-octanol

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A mixture of 5.0 g of 4-(trifluoromethoxy)phenol, 5.87 g of 8-bromo-1-octanol, and 7.76 g of K2CO3 in 56 ml of anhydrous dimethylformamide is stirred and heated at 80° C. for 16 hours. The reaction mixture is poured into dilute HCl solution and the mixture is extracted three times with ethyl acetate. The combined extracts are washed with brine and dried over MgSO4. After filtration and concentration, the crude product is purified by flash chromatography on silica gel, eluting with a 4:1 hexane/ethyl acetate mixture to give the title compound 8-(4-(trifluoromethoxy)-phenoxy)-1-octanol.

後処理

  1. extractionthe mixture is extracted three times with ethyl acetate
  2. washThe combined extracts are washed with brine
  3. dry with materialdried over MgSO4
  4. filtrationAfter filtration and concentration
  5. customthe crude product is purified by flash chromatography on silica gel
  6. washeluting with a 4:1 hexane/ethyl acetate mixture

出典と根拠

ORDレコード
ord-fba9e0b4c43c4132924eb337ae50aa28
出典データセット
uspto-grants-1996_05
特許番号
US05516767

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