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

HRID 1276824

反応式

HRID 1276824 の反応式
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]

参加物

5

反応物 3

HCID 66611,3-Dimethyl-2-imidazolidinone2 回HCID 14798Sodium HydroxideHCID 3029322,3,4-Trifluorobenzoic acid

生成物 1

HCID 27582863,4-Difluoro-2-hydroxybenzoic acid収率 95.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-210d2c0213b541a2adb95534b5747799
出典データセット
uspto-grants-2000_12
特許番号
US06166246

関連ノート

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