Potassium Carbonate → Ethyl 7-(4-acetonyl-1-piperazinyl)-6-fluoro-1-methyl-4-oxo-4H-(1,3)thiazeto(3,2-a)quinoline-3-carboxylate

HRID 1905430ノート

反応式

HRID 1905430 の反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1)[N:8]1[CH:18]([CH3:20])[S:19][C:7]1=[C:6]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:5]2=[O:26].C(=O)([O-])[O-].[K+].[K+].Br[CH2:34][C:35](=[O:37])[CH3:36]>CN(C)C=O>[CH2:34]([N:15]1[CH2:16][CH2:17][N:12]([C:11]2[CH:10]=[C:9]3[C:4]([C:5](=[O:26])[C:6]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[C:7]4[S:19][CH:18]([CH3:20])[N:8]43)=[CH:3][C:2]=2[F:1])[CH2:13][CH2:14]1)[C:35]([CH3:36])=[O:37]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 11715BromoacetoneHCID 10249018Ethyl 6-fluoro-1-methyl-4-oxo-7-(piperazin-1-yl)-1,4-dihydro-[1,3]thiazeto[3,2-a]quinoline-3-carboxylate

生成物 1

HCID 10002979Ethyl 7-(4-acetonyl-1-piperazinyl)-6-fluoro-1-methyl-4-oxo-4H-(1,3)thiazeto(3,2-a)quinoline-3-carboxylate収率 84.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Ethyl 6-fluoro-1-methyl-7-(1-piperazinyl)-4-oxo-4H-(1,3)thiazeto(3,2-a)quinoline-3-carboxylate (3.8 g) was suspended in 50 ml of N,N-dimethylformamide, 1.66 g of potassium carbonate was added thereto, 1.65 g of bromoacetone was dropped in with ice cooling and stirring, and the mixture was stirred at room temperature for 20 hours. The reaction solution was poured over into ice water and the crystals separated out were collected by filtration, washed with water, dried and recrystallized from ethanol to give 3.7 g of desired compound in colorless powdery crystals, m.p. 196°-200° C. (decompn.).

後処理

  1. stirringthe mixture was stirred at room temperature for 20 hours
  2. customthe crystals separated out
  3. filtrationwere collected by filtration
  4. washwashed with water
  5. customdried
  6. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-462c230f94fd418fb8cc10a9dffeec41
出典データセット
uspto-grants-1989_06
特許番号
US04843070

反応ノート

読み込み中…