Water → Ethyl 1-cyclopropyl-6,7-difluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylate

HRID 330084노트

반응식

HRID 330084 반응식
[H-].[Na+].F[C:4]1[C:22]([CH3:23])=[C:21]([F:24])[C:20]([F:25])=[CH:19][C:5]=1[C:6]([C:8](=[CH:14][NH:15][CH:16]1[CH2:18][CH2:17]1)[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:7].O>O1CCOCC1>[CH:16]1([N:15]2[C:4]3[C:5](=[CH:19][C:20]([F:25])=[C:21]([F:24])[C:22]=3[CH3:23])[C:6](=[O:7])[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:14]2)[CH2:18][CH2:17]1

참가 물질

5

반응물 3

HCID 962WaterHCID 24758Sodium hydrideHCID 178471874HCID 178471874, 화합물

생성물 1

HCID 9839540Ethyl 1-cyclopropyl-6,7-difluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylate수율 78.1%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To the cooled mixture of 55% sodium hydride (50 mg) in anhydrous dioxane (2 ml) was added ethyl 2-(2,4,5-trifluoro-3-methylbenzoyl)-3-cyclopropylaminoacrylate (300 mg) slowly with stirring. After stirring for 30 minutes at room temperature, to the reacting mixture was added water (5 ml), the resulting precipitate was collected by filtration, washed with water and recrystallized from methanol to give the title compound (220 mg) as white needles.

후처리

  1. stirringAfter stirring for 30 minutes at room temperature, to the reacting mixture
  2. filtrationthe resulting precipitate was collected by filtration
  3. washwashed with water
  4. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-095093658f054b148a2624a9d48df6a1
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04894458

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