Hydrochloric Acid → 7-Amino-1-(1-piperazinyl)-naphthalene

HRID 235151ノート

反応式

HRID 235151 の反応式
C([NH:9][C:10]1[CH:19]=[C:18]2[C:13]([CH:14]=[CH:15][CH:16]=[C:17]2[N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)=[CH:12][CH:11]=1)(=O)C1C=CC=CC=1.Cl>C(O)C>[NH2:9][C:10]1[CH:19]=[C:18]2[C:13]([CH:14]=[CH:15][CH:16]=[C:17]2[N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)=[CH:12][CH:11]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 189675377-Benzamido-1-(1-piperazinyl)-naphthalene2 回

生成物 1

HCID 189675327-Amino-1-(1-piperazinyl)-naphthalene収率 47%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The product of Example 11 (7-benzamido-1-(1-piperazinyl)-naphthalene, (0.063 g, 0.19 mmol) was combined with hydrochloric acid in ethanol (4 mL) and refluxed 16 hours. The reaction was concentrated at reduced pressure and the residue was neutralized with 4 N sodium hydroxide and extracted with methylene chloride. The organic phase was washed with brine, dried and concentrated to a tan solid (0.041 g). The solid was recrystallized from ethyl acetate/hexane to give 0.020 g (47%) of the title compound as light tan crystals. mp 184°-186° C. HRMS m/e calculated for C14H17N3 : 227.1419. Observed m/e 227.1405.

後処理

  1. temperaturerefluxed 16 hours
  2. concentrationThe reaction was concentrated at reduced pressure
  3. extractionextracted with methylene chloride
  4. washThe organic phase was washed with brine
  5. customdried
  6. concentrationconcentrated to a tan solid (0.041 g)
  7. customThe solid was recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-ba7fe15075624f5d973b232c3674cecf
出典データセット
uspto-grants-1997_01
特許番号
US05597826

反応ノート

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