Ammonia → 5-Methyl-2-(3-pyridyl)-thiazole
반응식
[C:1]([CH2:4][NH:5][C:6](=O)[C:7]1[CH:12]=[CH:11][CH:10]=[N:9][CH:8]=1)(=O)[CH3:2].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:15].N.C>C1(C)C=CC=CC=1>[CH3:2][C:1]1[S:15][C:6]([C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)=[N:5][CH:4]=1참가 물질
6
실험 절차
To a solution of 8.0 g (0.045 mol) of 73 in 125 ml of toluene, 10 g (0.045 mol) of P4S10 was added. The suspension was refluxed for 4 h and left at room temperature overnight. The mixture was poured into ice water followed by basification with ammonia. The two-phase system was stirred with charcoal and filtered. The toluene phase was separated and the aqueous phase extracted with 2×100 ml of toluene. The combined organic phases were dried over MgSO4 and evaporated in vacuo leaving a heavy, yellow oil, 88. Yield: 2.3 g (0.013 mol), 29%).
후처리
- temperatureThe suspension was refluxed for 4 h
- filtrationfiltered
- customThe toluene phase was separated
- extractionthe aqueous phase extracted with 2×100 ml of toluene
- dry with materialThe combined organic phases were dried over MgSO4
- customevaporated in vacuo
- customleaving a heavy, yellow oil, 88
출처 및 근거
- ORD 기록
- ord-8181380878094ce0ab0506052f44a5f2
- 출처 데이터셋
- uspto-grants-1989_09
- 특허 번호
- US04866077
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