1-Methylpiperazine → Hydrochloric Acid

HRID 652053ノート

反応式

HRID 652053 の反応式
[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]

参加物

6

反応物 2

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

生成物 2

HCID 313Hydrochloric AcidHCID 13041907HCID 13041907、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-126ee4a8f56c4d7d953660c171e2ab19
出典データセット
uspto-grants-1987_06
特許番号
US04670444

反応ノート

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