Chlorine → HCID 12733914、化合物

HRID 1578257ノート

反応式

HRID 1578257 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1Cl)[N:8]([CH2:13][CH3:14])[CH:7]=[C:6]([C:15]([OH:17])=[O:16])[C:5]2=[O:18].[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1.ClCl>COCCO.CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N:23]1[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]1)[N:8]([CH2:13][CH3:14])[CH:7]=[C:6]([C:15]([OH:17])=[O:16])[C:5]2=[O:18]

参加物

6

反応物 3

HCID 24526ChlorineHCID 531671-MethylpiperazineHCID 127338866,7-Dichloro-1-ethyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

生成物 1

HCID 12733914HCID 12733914、化合物収率 53%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 80192-Methoxyethanol溶媒

実験手順

A solution of 4.3 g (0.015 mol) of 6,7-dichloro-1-ethyl-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid and 9 g of 1-methylpiperazine in a mixture of methyl cellosolve (45 cm3) and dimethylformamide (10 cm3) was heated to reflux temperature. After 6 hours, 75% of the theoretical amount of ionized chlorine (1 atom) had been released into the mixture. Heating was continued for a further 2 hours. The solution was concentrated to dryness in vacuo. The residue was taken up in 20 cm3 of ethanol. The solid, which was filtered off and recrystallised from methyl cellosolve, gave 2.78 g of 6-chloro-1-ethyl-7-(4-methylpiperazinyl)-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid, m.p. 260° C., which was identical to the compound described in Example 1.

後処理

  1. temperaturewas heated
  2. temperatureto reflux temperature
  3. temperatureHeating
  4. waitwas continued for a further 2 hours
  5. concentrationThe solution was concentrated to dryness in vacuo
  6. filtrationThe solid, which was filtered off
  7. customrecrystallised from methyl cellosolve

出典と根拠

ORDレコード
ord-f389cab282ec4b5da1a5ce97f6951e82
出典データセット
uspto-grants-1981_09
特許番号
US04292317

反応ノート

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