Water → HCID 178524533, 화합물

HRID 246934노트

반응식

HRID 246934 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 178524533HCID 178524533, 화합물수율 93.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-997d3c6621cb492bae00fb53c71f0f09
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04704459

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