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Piperidine → 9-chloro-8-(1-piperidyl)-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid

HRID 1583618
ノート
印刷プレビュー

反応式

HRID 1583618 の反応式
Cl[C:2]1[C:13]2=[C:14]3[N:9]([CH:10]([CH3:15])[CH2:11][CH2:12]2)[CH:8]=[C:7]([C:16]([OH:18])=[O:17])[C:6](=[O:19])[C:5]3=[CH:4][C:3]=1[Cl:20].[NH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1>CN(C)P(=O)(N(C)C)N(C)C>[Cl:20][C:3]1[CH:4]=[C:5]2[C:14]3[N:9]([CH:8]=[C:7]([C:16]([OH:18])=[O:17])[C:6]2=[O:19])[CH:10]([CH3:15])[CH2:11][CH2:12][C:13]=3[C:2]=1[N:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8082Piperidine2 回HCID 155717798,9-dichloro-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid

生成物 1

HCID 130442959-chloro-8-(1-piperidyl)-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid収率 24.4%

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒2 回

実験手順

In a 200 ml autoclave were placed 4.6 g of 8,9-dichloro-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid, 5 g of piperidine and 50 ml of hexamethylphosphoric triamide and the mixture was reacted at 160° C. on an oil bath for 5 hours. After completion of reaction hexamethylphosphoric triamide and piperidine were distilled off under reduced pressure and to the residue was added ethyl acetate and crystallized. Recrystallization from dimethylformamide-water gave 1.3 g of 9-chloro-8-(1-piperidyl)-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid. m.p. 246° to 248° C.

後処理

  1. customthe mixture was reacted at 160° C. on an oil bath for 5 hours
  2. distillationwere distilled off under reduced pressure and to the residue
  3. additionwas added ethyl acetate
  4. customcrystallized
  5. customRecrystallization from dimethylformamide-water

出典と根拠

ORDレコード
ord-9bebc97cd311465498b5801d1fedf48e
出典データセット
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04552879

反応ノート

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