Nitric Acid → 2-Nitro-4-(trifluoromethoxy)phenol

HRID 884950

反応式

HRID 884950 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.[N+:13]([O-])([OH:15])=[O:14]>C(O)(=O)C>[F:1][C:2]([F:11])([F:12])[O:3][C:4]1[CH:5]=[CH:6][C:7]([OH:10])=[C:8]([N+:13]([O-:15])=[O:14])[CH:9]=1

参加物

4

反応物 2

HCID 944Nitric AcidHCID 70015p-(Trifluoromethoxy)phenol

生成物 1

HCID 27757752-Nitro-4-(trifluoromethoxy)phenol収率 90.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a mixture of 4.0 g of 4-trifluoromethoxy phenol and 25 ml of acetic acid, a mixture of 2.02 g of 70% nitric acid and 10 ml of acetic acid was added dropwise with the temperature kept at 10-15° C. The reaction mixture was stirred for five hours. The reaction mixture was poured into ice water and extracted with ethyl acetate. The combined organic layers were washed with water, a saturated aqueous solution of sodium hydrogencarbonate and a saturated sodium chloride solution, dried over sodium sulfate, and then concentrated under reduced pressure to give 4.53 g of 4-trifluoromethoxy-2-nitrophenol.

後処理

  1. additionwas added dropwise with the temperature
  2. customkept at 10-15° C
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layers were washed with water
  5. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and a saturated sodium chloride solution, dried over sodium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-767b58711ffb407e8e79b774426b196a
出典データセット
uspto-grants-2012_08
特許番号
US08242133B2

関連ノート

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