Sodium Carbonate → 2-Methylthiazolo[5,4-b]pyridine
反応式
P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:2].C([O-])([O-])=O.[Na+].[Na+].[C:21]([NH:24][C:25]1[C:26](Cl)=[N:27][CH:28]=[CH:29][CH:30]=1)(=O)[CH3:22].[OH-].[Na+]>C1COCC1>[CH3:22][C:21]1[S:2][C:26]2[C:25]([N:24]=1)=[CH:30][CH:29]=[CH:28][N:27]=2参加物
6
実験手順
Phosphorus pentasulfide (56.5 g) and Na2CO3 (13.7 g) were mixed together in 400 mL of THF for ~30 min. To this solution, a solution of the product of Step 1 (17.32 g) in 100 mL of THF was added and the mixture was stirred at room temperature overnight. 2M NaOH (500 mL) was added and the mixture was stirred at room temperature for 2 hr. The product was extracted in EtOAc, washed with brine, dried over Na2SO4, and purified by flash chromatography on silica with EtOAc: toluene 20:80; yield: 12.07 g, (83%).
後処理
- stirringthe mixture was stirred at room temperature for 2 hr
- extractionThe product was extracted in EtOAc
- washwashed with brine
- dry with materialdried over Na2SO4
- custompurified by flash chromatography on silica with EtOAc: toluene 20:80
出典と根拠
- ORDレコード
- ord-4f7276a965f24679ae00e039e90563e7
- 出典データセット
- uspto-grants-1995_12
- 特許番号
- US05472964
反応ノート
読み込み中…