1-Methylpiperazine → Hydrochloric Acid

HRID 652053노트

반응식

HRID 652053 반응식
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:18])[C:7]([C:15]([OH:17])=[O:16])=[CH:8][N:9]2[CH:12]2[CH2:14][CH2:13]2)=[CH:4][N:3]=1.[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>C(O)C.CS(C)=O>[CH3:19][N:20]1[CH2:25][CH2:24][N:23]([C:2]2[CH:11]=[C:10]3[C:5]([C:6](=[O:18])[C:7]([C:15]([OH:17])=[O:16])=[CH:8][N:9]3[CH:12]3[CH2:14][CH2:13]3)=[CH:4][N:3]=2)[CH2:22][CH2:21]1.[ClH:1]

참가 물질

6

반응물 2

HCID 531671-MethylpiperazineHCID 130419067-Chloro-1-cyclopropyl-4-oxo-1,4-dihydro-1,6-naphthyridine-3-carboxylic acid

생성물 2

HCID 313Hydrochloric AcidHCID 13041907HCID 13041907, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 702Ethanol용매

실험 절차

A suspension of 2.64 g of 7-chloro-1-cyclopropyl-4-oxo-1,4-dihydro-1,6-naphthyridine-3-carboxylic acid and 2.5 g of N-methylpiperazine in 30 ml of ethanol or DMSO (=Dimethylsulfoxide) was heated to the boiling point under reflux for 16 hours or to 135°-140° C. for two hours. The diluent was distilled off in vacuo, the residue was dissolved in 30 ml of 1N NaOH, the solution was filtered and the filtrate was acidified with 10 strength hydrochloric acid. The precipitate was filtered off and washed with water and ethanol. It could be recrystallised from N-dimethylformamide/ethanol. 3.1 g (94% of the theoretical yield) of 7-(4-methylpiperazino)-1-cyclopropyl-4-oxo-1,4-dihydro-1,6-naphthyridine-3-carboxylic acid of melting point 326° C. (hydrochloride) (decomposition) were obtained.

후처리

  1. temperaturewas heated to the boiling point
  2. temperatureunder reflux for 16 hours or to 135°-140° C. for two hours
  3. distillationThe diluent was distilled off in vacuo
  4. dissolutionthe residue was dissolved in 30 ml of 1N NaOH
  5. filtrationthe solution was filtered
  6. filtrationThe precipitate was filtered off
  7. washwashed with water and ethanol
  8. customIt could be recrystallised from N-dimethylformamide/ethanol

출처 및 근거

ORD 기록
ord-126ee4a8f56c4d7d953660c171e2ab19
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04670444

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