Ethanol → HCID 178423444, 화합물

HRID 916082노트

반응식

HRID 916082 반응식
[C:1]1([CH2:11][NH:12][C:13]2[CH:18]=C[C:16](C)=[CH:15][C:14]=2[NH2:20])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[SH-:21].[C+4:22].[SH-].[SH-].[SH-].[CH2:26](O)[CH3:27]>>[C:1]1([CH2:11][N:12]2[C:13]3[CH:18]=[C:26]([CH3:27])[CH:16]=[CH:15][C:14]=3[N:20]=[C:22]2[SH:21])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 3

HCID 702EthanolHCID 17810729((1-Naphthyl)methyl)(2-amino-4-methyl-phenyl)amineHCID 178420937HCID 178420937, 화합물

생성물 1

HCID 178423444HCID 178423444, 화합물수율 44%

실험 절차

Subsequently, ((1-naphthyl)methyl)(2-amino-4-methyl-phenyl)amine (943.1 mg, 3.59 mmol) was dissolved in ethanol (6.4 ml), to which carbon bisulfide (7 ml, 116 mmol) was added, and then refluxed. After 10 hours, it was returned to room temperature, concentrated under reduced pressure. Ethanol (2 ml) was added to the residue, which was stirred at room temperature for 30 minutes, and was further stirred on ice for 30 minutes. The resulting crystals were filtered, and dried to obtain 1-((1-naphthyl)methyl)-6-methyl-benzimidazole-2-thiol (459.1 mg, yield 44%, 2 steps).

후처리

  1. additionwas added
  2. temperaturerefluxed
  3. customwas returned to room temperature
  4. concentrationconcentrated under reduced pressure
  5. additionEthanol (2 ml) was added to the residue, which
  6. stirringwas further stirred on ice for 30 minutes
  7. filtrationThe resulting crystals were filtered
  8. customdried

출처 및 근거

ORD 기록
ord-24e62a9e4c214738bfaf1dc9e2a399eb
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07268145B2

반응 노트

불러오는 중…