Dimethylformamide → HCID 20427616、化合物

HRID 615332ノート

反応式

HRID 615332 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:20])[C:7]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:8][N:9]2NC=O)=[CH:4][C:3]=1[F:21].[C:22](=[O:25])([O-])[O-].[K+].[K+].CI.[CH3:30][N:31](C)C=O>>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:20])[C:7]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:8][NH:9]2)=[C:4]([NH:31][CH2:30][CH:22]=[O:25])[C:3]=1[F:21]

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 3021289[7-Chloro-3-(ethoxycarbonyl)-6-fluoro-4-oxoquinolin-1(4H)-yl]methanimidic acid

生成物 1

HCID 20427616HCID 20427616、化合物

反応条件

温度
25 °C

実験手順

A mixture of 14.65 g (0.047 mole) of ethyl 7-chloro-6-fluoro-1-(formylamino)-1,4-dihydro-4-oxo-3-quinolinecarboxylate (Preparation 2), 12.9 g (0.094 mole) of potassium carbonate and 200 ml of dimethylformamide was stirred at 25° C. for 90 minutes. Methyl iodide (20.0 g, 0.141 mole) was then added and the reaction mixture was stirred at room temperature for 90 minutes. The dimethylformamide was removed in high vacuum at 50° C., and the residue was partitioned between 250 ml of water and 500 ml of chloroform. The chloroform layer was separated and dried over anhydrous magnesium sulfate. There was obtained from the chloroform solution upon concentration 13.8 g of ethyl 7-chloro-6-fluoro-1,4-dihydro-5-[(formyl)methylamino]-4-oxo-3-quinolinecarboxylate, m.p. 213°-216° C.

後処理

  1. stirringthe reaction mixture was stirred at room temperature for 90 minutes
  2. customThe dimethylformamide was removed in high vacuum at 50° C.
  3. customthe residue was partitioned between 250 ml of water and 500 ml of chloroform
  4. customThe chloroform layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate

出典と根拠

ORDレコード
ord-e95da60994f24d97ad839b4f273b6b29
出典データセット
uspto-grants-1985_02
特許番号
US04499091

反応ノート

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