Hydrochloric Acid → HCID 178430974、化合物

HRID 1700537ノート

反応式

HRID 1700537 の反応式
[CH3:1][S:2]([N:5]1[C:13]2[CH2:12][CH:11]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:10][C:9](=O)[C:8]=2[C:7]([CH3:21])=[CH:6]1)(=[O:4])=[O:3].[C:22]([NH:25][NH2:26])([NH2:24])=[NH:23].[ClH:27].Cl.O>C(O)C>[ClH:27].[NH:25]([N:26]=[C:9]1[CH2:10][CH:11]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:12][C:13]2[N:5]([S:2]([CH3:1])(=[O:4])=[O:3])[CH:6]=[C:7]([CH3:21])[C:8]1=2)[C:22]([NH2:24])=[NH:23]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 18317470HCID 18317470、化合物HCID 178418668HCID 178418668、化合物

生成物 1

HCID 178430974HCID 178430974、化合物収率 46.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1-methanesulfonyl-3-methyl-6-phenyl-4,5,6,7-tetrahydroindol-4-one (0.41 g), aminoguanidine hydrochloride (0.16 g), concentrated hydrochloric acid (0.068 ml), water (0.068 ml) and ethanol (30 ml) was refluxed for 20 minutes. The reaction solution was allowed to stand in a refrigerator for 12 hours, and precipitated crystals were filtered, which were washed with ethanol and recrystallized from water to give 4-guanidinoimino-1-methanesulfonyl-3-methyl-6-phenyl-4,5,6,7-tetrahydroindole hydrochloride (Compound 13) (0.25 g) as colorless crystals.

後処理

  1. temperaturewas refluxed for 20 minutes
  2. customprecipitated crystals
  3. filtrationwere filtered
  4. washwhich were washed with ethanol
  5. customrecrystallized from water

出典と根拠

ORDレコード
ord-07ed04ea9a6644dbbf0249f011d8004f
出典データセット
uspto-grants-2002_02
特許番号
US06350749B1

反応ノート

読み込み中…