Ammonia → 5-Methyl-2-(3-pyridyl)-thiazole
反応式
[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]=1参加物
6
実験手順
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 phase were dried over MgSO4 and evaporated in vacuo leaving a heavy, yellow oil, 88. Yield: 2.3 g (0.013 mol), 29%).
後処理
- 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 phase were dried over MgSO4
- customevaporated in vacuo
- customleaving a heavy, yellow oil, 88
出典と根拠
- ORDレコード
- ord-dddecb71856e4b40b10c34c0a9991333
- 出典データセット
- uspto-grants-1999_11
- 特許番号
- USRE036374
反応ノート
読み込み中…