Phosphorus oxide (P4O10) → 4-Oxo-4,5,6,7-tetrahydrothieno-(3,2-C)pyridine
반응식
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]1참가 물질
4
반응 조건
- 온도
- 110 °C
실험 절차
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).
후처리
- customto afford the crude product
- customPurification by column chromatography on silica gel (2% methanol in CHCl3)
출처 및 근거
- ORD 기록
- ord-375c703fe5ff4d3ca211665eb22edbee
- 출처 데이터셋
- uspto-grants-2015_02
- 특허 번호
- US08946260B2
반응 노트
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