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

HRID 330084ノート

反応式

HRID 330084 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 24758Sodium hydrideHCID 178471874HCID 178471874、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-095093658f054b148a2624a9d48df6a1
出典データセット
uspto-grants-1990_01
特許番号
US04894458

反応ノート

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