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Benzyl Alcohol → 4-(Benzyloxy)-3-(trifluoromethyl)benzoic acid

HRID 1093490
ノート
印刷プレビュー

反応式

HRID 1093490 の反応式
CC(C)([O-])C.[K+].[CH2:7]([OH:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.F[C:16]1[CH:24]=[CH:23][C:19]([C:20]([OH:22])=[O:21])=[CH:18][C:17]=1[C:25]([F:28])([F:27])[F:26].Cl>CN(C)C=O>[CH2:7]([O:14][C:16]1[CH:24]=[CH:23][C:19]([C:20]([OH:22])=[O:21])=[CH:18][C:17]=1[C:25]([F:26])([F:28])[F:27])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 244Benzyl AlcoholHCID 313Hydrochloric AcidHCID 5222684-Fluoro-3-(trifluoromethyl)benzoic acidHCID 23665647Potassium tert-butoxide

生成物 1

HCID 167490234-(Benzyloxy)-3-(trifluoromethyl)benzoic acid

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

実験手順

To a solution of potassium t-butoxide (27.5 g) in N,N-dimethylformamide (120 ml) was added dropwise a solution of benzyl alcohol (15.9 ml) in N,N-dimethylformamide (60 ml) over min. The mixture was stirred for 30 min, and a solution of 4-fluoro-3-trifluoromethylbenzoic acid (20.0 g) in N,N-dimethylformamide (90 ml) was added under ice-cooling. The mixture was stirred at room temperature for 1 hr, and further at 50° C. for 1 hr. The reaction mixture was added to ice water, and acidified with 1M hydrochloric acid (300 ml). The precipitated solid was collected by filtration, and washed with water and then hexane to give the object product (28.2 g) as a white powder.

後処理

  1. temperaturecooling
  2. stirringThe mixture was stirred at room temperature for 1 hr
  3. waitfurther at 50° C. for 1 hr
  4. filtrationThe precipitated solid was collected by filtration
  5. washwashed with water

出典と根拠

ORDレコード
ord-d17a7f01b4804136b4d732fa17f78b88
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08129361B2

反応ノート

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