Hydrochloric Acid → 2-Nitro-4-(trifluoromethyl)phenol

HRID 28246

反応式

HRID 28246 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[Cl-].C(CCCCCCCCCCCC[NH+](C)C)C1C=CC=CC=1.[OH-:38].[K+].Cl>COCCO>[N+:12]([C:3]1[CH:4]=[C:5]([C:8]([F:11])([F:10])[F:9])[CH:6]=[CH:7][C:2]=1[OH:38])([O-:14])=[O:13]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 84624-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotolueneHCID 14797Potassium HydroxideHCID 53445721Benzyldodecyldimethyl ammonium chloride

生成物 1

HCID 98162-Nitro-4-(trifluoromethyl)phenol収率 92%

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

反応条件

温度
65 °C

実験手順

45 g of 4-chloro-3-nitro-benzotrifluoride and 10 ml of 50% strength aqueous benzyldodecyldimethylammonium chloride are initially introduced into 150 ml of ethylene glycol monomethyl ether, and 100 g of 50% strength potassium hydroxide solution are added dropwise in the course of about 30 minutes, up to a temperature of 65° C. The mixture is then stirred at 65° C. for 6 hours and subsequently cooled and rendered acid with concentrated hydrochloric acid, and about 500 ml of distillate are driven over with steam. The organic phase is separated off and washed with 20 ml of dilute hydrochloric acid, and the organic phase is again separated off and dried with sodium sulphate. 38 g of 2-nitro-4-trifluoromethylphenol are obtained, which corresponds to a yield of 92% of theory.

後処理

  1. additionare added dropwise in the course of about 30 minutes, up to a temperature of 65° C
  2. temperaturesubsequently cooled
  3. customThe organic phase is separated off
  4. washwashed with 20 ml of dilute hydrochloric acid
  5. customthe organic phase is again separated off
  6. dry with materialdried with sodium sulphate

出典と根拠

ORDレコード
ord-dd14553770ba48f4a69e66321c63b24e
出典データセット
uspto-grants-1980_09
特許番号
US04225731

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