Triethylamine → HCID 178485206, 화합물

HRID 1491860노트

반응식

HRID 1491860 반응식
Cl.Cl.Cl.[NH2:4][CH2:5][C:6]1[N:11]=[C:10]([C:12]2[N:13]=[C:14]([N:17]=[C:18]([NH2:20])[NH2:19])[S:15][CH:16]=2)[CH:9]=[CH:8][CH:7]=1.[CH2:21]([N:23]([CH2:26]C)CC)C.[CH3:28][S:29]([N:32]=C(SC)SC)(=[O:31])=[O:30]>C(O)C>[NH2:19][C:18](=[N:17][C:14]1[S:15][CH:16]=[C:12]([C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([CH2:5][NH:4][C:21]([NH:23][CH3:26])=[N:32][S:29]([CH3:28])(=[O:31])=[O:30])[N:11]=2)[N:13]=1)[NH2:20]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 13449843N-[bis(methylsulfanyl)methylidene]methanesulfonamideHCID 189538374-(6-Aminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole trihydrochloride

생성물 1

HCID 178485206HCID 178485206, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 4-(6-aminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole trihydrochloride (1.5 g), triethylamine (1.8 ml) and dimethyl N-methanesulfonyl-dithiocarbonimidate (0.8 g) in ethanol (30 ml) was heated under reflux for 5 hours. The solvent was removed by concentration in vacuo. To the residue was added to a mixture of 40% aqueous methylamine (4.0 ml) in N,N-dimethylformamide (13 ml) and the mixture was stirred at ambient temperature for 30 hours. The reaction mixture was added a water and the isolated precipitate was collected by filtration to give 2-(diaminomethyleneamino)-4-[6-(2-methanesulfonyl-3-methylguanidino)methylpyridin-2-yl]thiazole (1.12 g).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. customThe solvent was removed by concentration in vacuo
  4. additionTo the residue was added to a mixture of 40% aqueous methylamine (4.0 ml) in N,N-dimethylformamide (13 ml)
  5. additionThe reaction mixture was added a water
  6. filtrationthe isolated precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-3c3b36523e494eee9cca01f39a42c768
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05371097

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