反応式
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10]1[C:11]([Cl:30])=[N:12][C:13]([CH:17]2[CH2:22][CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18]2)=[N:14][C:15]=1[OH:16].Cl>CO>[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10]1[C:15]([OH:16])=[N:14][C:13]([CH:17]2[CH2:18][CH2:19][NH:20][CH2:21][CH2:22]2)=[N:12][C:11]=1[Cl:30]参加物
4
実験手順
Into a solution of tert-butyl 4-[5-(1,3-benzothiazol-2-yl)-4-chloro-6-hydroxypyrimidin-2-yl]piperidine-1-carboxylate (44.7 g, 100.01 mmol, 1.00 equiv) in methanol (50 ml) was added concentrated hydrochloric acid (50 mL, 12 M). The resulting solution was stirred for 30 min at room temperature. Concentration under vacuum gave 34 g of 5-(1,3-benzothiazol-2-yl)-6-chloro-2-(piperidin-4-yl)pyrimidin-4-ol as a yellow solid, which was used directly for next step without further purification. MS m/z [M+H](ESI): 347.
後処理
- concentrationConcentration under vacuum
出典と根拠
- ORDレコード
- ord-bd1135f847474bb9bc2305e9ca91e855
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09221809B2
関連ノート
読み込み中…