Methyl 3-cyano-2,4,5-trifluoro-benzoate → 195532-64-0

HRID 367014ノート

反応式

HRID 367014 の反応式
[C:1]([C:3]1[C:4]([F:15])=[C:5]([CH:10]=[C:11]([F:14])[C:12]=1[F:13])[C:6]([O:8]C)=[O:7])#[N:2]>C(O)(=O)C.O.S(=O)(=O)(O)O>[C:1]([C:3]1[C:4]([F:15])=[C:5]([CH:10]=[C:11]([F:14])[C:12]=1[F:13])[C:6]([OH:8])=[O:7])#[N:2]

参加物

5

反応物 1

HCID 18417526Methyl 3-cyano-2,4,5-trifluoro-benzoate

生成物 1

HCID 18417533195532-64-0収率 81.3%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 962Water溶媒HCID 1118Sulfuric Acid溶媒

実験手順

A solution of 156 g of methyl 3-cyano-2,4,5-trifluoro-benzoate in 960 ml of glacial acetic acid, 140 ml of water and 69 ml of concentrated sulphuric acid is heated to reflux for 8 hours. The acetic acid is then largely removed by distillation in vacuo and the residue is treated with water. The precipitated solid is filtered off with suction, washed with water and dried. 118.6 g of 3-cyano-2,4,5-trifluoro-benzoic acid are obtained as a white solid of melting point 187-190° C.

後処理

  1. temperatureto reflux for 8 hours
  2. customThe acetic acid is then largely removed by distillation in vacuo
  3. additionthe residue is treated with water
  4. filtrationThe precipitated solid is filtered off with suction
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-76c93e836d2145519411fcf0082963d5
出典データセット
uspto-grants-2000_10
特許番号
US06133260

反応ノート

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