Lawesson's reagent → HCID 57973784, 화합물
반응식
[F:1][C:2]([F:14])([F:13])[C:3]1[N:7]2[CH2:8][CH2:9][NH:10][C:11](=O)[C:6]2=[N:5][N:4]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:24])=CC=1>>[F:1][C:2]([F:14])([F:13])[C:3]1[N:7]2[CH2:8][CH2:9][NH:10][C:11](=[S:24])[C:6]2=[N:5][N:4]=1참가 물질
3
실험 절차
A mixture of 173 mg (0.84 mmol) of 3-(trifluoromethyl)-6,7-dihydro[1,2,4]triazolo[4,3-a]pyrazin-8(5H)-one, 703 mg (1.68 mmol) of Lawesson's Reagent, and 18 mL of xylenes was stirred at reflux for 4.5 h. After being cooled to room temperature, the solvent was decanted off, and the residue was washed with diethyl ether. The resulting solid was dried and purified by flash chromatography (20-50% acetone in hexanes) to give the title compound as a greenish-yellow solid. LC-MS 223 (M+1).
후처리
- temperatureat reflux for 4.5 h
- customthe solvent was decanted off
- washthe residue was washed with diethyl ether
- customThe resulting solid was dried
- custompurified by flash chromatography (20-50% acetone in hexanes)
출처 및 근거
- ORD 기록
- ord-2b6cf08764ab4a38a980079c14365388
- 출처 데이터셋
- uspto-grants-2009_12
- 특허 번호
- US07625888B2
반응 노트
불러오는 중…