Hydrochloric Acid → HCID 22407929、化合物

HRID 36138

反応式

HRID 36138 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 22407929HCID 22407929、化合物

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-a10137d50be249069508be380a70b375
出典データセット
uspto-grants-1995_05
特許番号
US05412137

関連ノート

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