1,3-Dimethyl-2-imidazolidinone → 3,4-Difluoro-2-hydroxybenzoic acid

HRID 1276824

반응식

HRID 1276824 반응식
F[C:2]1[C:10]([F:11])=[C:9]([F:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[OH-].[Na+].CN1CCN(C)C1=[O:22]>O>[F:11][C:10]1[C:9]([F:12])=[CH:8][CH:7]=[C:3]([C:4]([OH:6])=[O:5])[C:2]=1[OH:22]

참가 물질

5

반응물 3

HCID 66611,3-Dimethyl-2-imidazolidinone2회HCID 14798Sodium HydroxideHCID 3029322,3,4-Trifluorobenzoic acid

생성물 1

HCID 27582863,4-Difluoro-2-hydroxybenzoic acid수율 95.1%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

1.76 g (0.01 mole) of 2,3,4-trifluorobenzoic acid, 1.62 g (0.04 mole) of powdery 99% sodium hydroxide and 20 ml of 1,3-dimethyl-2-imidazolidinone were fed into a 100-ml four-necked flask provided with a thermometer, a stirrer and a reflux condenser. The mixture was stirred at 150° C. for 2 hours to give rise to a reaction. After the completion of the reaction, part of 1,3-dimethyl-2-imidazolidinone was recovered. The resulting reaction mixture was diluted with 500 ml of water and then subjected to precipitation with a 10% aqueous hydrochloric acid solution. The resulting material was cooled in an ice bath. The resulting crystals were collected by filtration, washed with water, and dried to obtain 1.66 g of 3,4-difluorosalicylic acid. The isolated yield was 95.1% relative to the 2,3,4-trifluorobenzoic acid used.

후처리

  1. customprovided with a thermometer, a stirrer and a reflux condenser
  2. customto give rise
  3. customto a reaction
  4. customwas recovered
  5. customThe resulting reaction mixture
  6. customsubjected to precipitation with a 10% aqueous hydrochloric acid solution
  7. temperatureThe resulting material was cooled in an ice bath
  8. filtrationThe resulting crystals were collected by filtration
  9. washwashed with water
  10. customdried

출처 및 근거

ORD 기록
ord-210d2c0213b541a2adb95534b5747799
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06166246

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