Hydrochloric Acid → HCID 178428136、化合物

HRID 49207ノート

反応式

HRID 49207 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH:9]1[CH2:18][C:17]2[N:16]=[CH:15][CH:14]=[C:13]([CH3:19])[C:12]=2[C:11](=O)[CH2:10]1.[C:21]([NH:24][NH2:25])([NH2:23])=[NH:22].[ClH:26].Cl.O>C(O)C>[ClH:26].[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH:9]1[CH2:18][C:17]2[N:16]=[CH:15][CH:14]=[C:13]([CH3:19])[C:12]=2[C:11](=[N:25][NH:24][C:21]([NH2:23])=[NH:22])[CH2:10]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 110869317-(2,5-Difluorophenyl)-4-methyl-5,6,7,8-tetrahydroquinolin-5-oneHCID 178418668HCID 178418668、化合物

生成物 1

HCID 178428136HCID 178428136、化合物収率 99.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 7-(2,5-difluorophenyl)-4-methyl-5,6,7,8-tetrahydroquinolin-5-one (1.2 g) and aminoguanidine hydrochloride (0.58 g) in ethanol (30 ml) was combined with concentrated hydrochloric acid (1.1 ml) and water (1.1 ml), and the mixture was heated under reflux for 14 hours. The solvent was distilled off under reduced pressure, and the resultant crystal was recrystallized from ethanol to obtain 7-(2,5-difluorophenyl)-5-guanidinoimino-4-methyl-5,6,7,8-tetrahydroquinoline hydrochloride (Compound K) (1.6 g) as a colorless crystal.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 14 hours
  3. distillationThe solvent was distilled off under reduced pressure
  4. customthe resultant crystal was recrystallized from ethanol

出典と根拠

ORDレコード
ord-4f1d164094b047a693bf9993ac9e2f7b
出典データセット
uspto-grants-2004_03
特許番号
US06706732B1

反応ノート

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