반응식
[C:1](S(O)=O)([NH2:3])=[NH:2].[H-].[Na+].[Na].N[CH2:11][CH2:12]S.[CH3:14][O-].[Na+].Cl.Cl.[NH2:19][CH2:20]CS.[CH3:23][S:24]([CH3:26])=O>CO.O>[NH2:19][CH2:20][CH2:23][S:24][CH2:26][C:14]1[N:2]=[CH:1][NH:3][C:11]=1[CH3:12]참가 물질
반응물 7
생성물 1
시약·촉매·용매 2
실험 절차
Triphenyl β-acetylvinylphosphonium bromide (4.11 g, 0.01 mole) was added in one portion to a stirred suspension of 1.1 g (0.01 mole) of formamidine sulfinic acid in 20 ml of dimethylsulfoxide containing 0.25 g of sodium hydride. The mixture was stirred at ambient temperature for 1 hour then at 80° for an additional hour. A solution of 0.99 g (0.01 mole) of the sodium salt of cysteamine, prepared by addition of two equivalents of sodium methoxide to cysteamine dihydrochloride, in 10 ml of methanol was added and the resulting mixture was heated at 70°-80° for 4 hours. The mixture was diluted with twice its volume of water and the triphenyl phosphine was removed by filtration. The filtrate was extracted with 100 ml of toluene and with two 100 ml portions of chloroform. The chloroform extracts were combined, dried and evaporated to dryness to give 4-(2-aminoethyl)thiomethyl-5-methylimidazole in 45% yield.
후처리
- waitat 80° for an additional hour
- additionwas added
- temperaturethe resulting mixture was heated at 70°-80° for 4 hours
- customthe triphenyl phosphine was removed by filtration
- extractionThe filtrate was extracted with 100 ml of toluene and with two 100 ml portions of chloroform
- customdried
- customevaporated to dryness
출처 및 근거
- ORD 기록
- ord-77e8e0a94005434c9bcf97a7ff593841
- 출처 데이터셋
- uspto-grants-1979_08
- 특허 번호
- US04163858
연결된 노트
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