Phosphorus oxide (P4O10) → 4-Oxo-4,5,6,7-tetrahydrothieno-(3,2-C)pyridine
反応式
C([O:3][C:4](=O)[NH:5][CH2:6][CH2:7][C:8]1[S:9][CH:10]=[CH:11][CH:12]=1)C.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O=P(Cl)(Cl)Cl>[S:9]1[C:8]2[CH2:7][CH2:6][NH:5][C:4](=[O:3])[C:12]=2[CH:11]=[CH:10]1参加物
4
反応条件
- 温度
- 110 °C
実験手順
Using an analogous procedure and workup as described in Example 1, step 4, (2-thiophen-2-yl-ethyl)-carbamic acid ethyl ester (I-7c: 800 mg, 3.50887 mmol) in POCl3 (10 mL) was reacted with P2O5 (996 mg, 7.0175 mmol). The resulting mixture was stirred at 110° C. for 4 hours to afford the crude product. Purification by column chromatography on silica gel (2% methanol in CHCl3) afforded 180 mg of the product (33.5% yield).
後処理
- customto afford the crude product
- customPurification by column chromatography on silica gel (2% methanol in CHCl3)
出典と根拠
- ORDレコード
- ord-375c703fe5ff4d3ca211665eb22edbee
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08946260B2
反応ノート
読み込み中…