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

HRID 367014노트

반응식

HRID 367014 반응식
[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]

참가 물질

5

반응물 1

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

생성물 1

HCID 18417533195532-64-0수율 81.3%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매HCID 1118Sulfuric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-76c93e836d2145519411fcf0082963d5
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06133260

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