Water → HCID 178524533、化合物

HRID 246934ノート

反応式

HRID 246934 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[N:19]=[C:18]([OH:20])[C:17]([F:21])=[CH:16][C:11]=1[C:12]([O:14]C)=[O:13].[OH-].[Na+].C(OCC)(=O)C.O>CO>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[N:19]=[C:18]([OH:20])[C:17]([F:21])=[CH:16][C:11]=1[C:12]([OH:14])=[O:13]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 178498343Methyl 2-(2,4-difluorophenylamino)-5-fluoro-6-hydroxynicotinate

生成物 1

HCID 178524533HCID 178524533、化合物収率 93.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 30 ml of methanol was suspended 3.00 g of methyl 2-(2,4-difluorophenylamino)-5-fluoro-6-hydroxynicotinate, and 16.1 ml of 2N aqueous sodium hydroxide solution was added thereto at room temperature, after which the resulting mixture was subjected to reaction under reflux for 4 hours. Subsequently, the reaction mixture was added to a mixture of 60 ml of ethyl acetate and 60 ml of water, and the aqueous layer was separated. The aqueous layer was adjusted to pH 1.0 with 6N hydrochloric acid, and the crystals thus deposited were collected by filtration, washed successively with 15 ml of water and 25 ml of isopropyl alcohol to obtain 2.68 g (yield 93.7%) of 2-(2,4-difluorophenylamino)-5-fluoro-6-hydroxynicotinic acid having a melting point of 213°-216° C.

後処理

  1. additionwas added
  2. customat room temperature, after which the resulting mixture was subjected to reaction
  3. temperatureunder reflux for 4 hours
  4. customthe aqueous layer was separated
  5. filtrationthe crystals thus deposited were collected by filtration
  6. washwashed successively with 15 ml of water and 25 ml of isopropyl alcohol

出典と根拠

ORDレコード
ord-997d3c6621cb492bae00fb53c71f0f09
出典データセット
uspto-grants-1987_11
特許番号
US04704459

反応ノート

読み込み中…