Chlorine → HCID 12733914, 화합물

HRID 1578257노트

반응식

HRID 1578257 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 12733914HCID 12733914, 화합물수율 53%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 80192-Methoxyethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f389cab282ec4b5da1a5ce97f6951e82
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04292317

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