Lawesson's reagent → 3,3,3-Trifluoro-2,2-dimethyl-thiopropionamide
반응식
[F:1][C:2]([F:10])([F:9])[C:3]([CH3:8])([CH3:7])[C:4]([NH2:6])=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:20])=CC=1>C1COCC1>[F:1][C:2]([F:10])([F:9])[C:3]([CH3:8])([CH3:7])[C:4]([NH2:6])=[S:20]참가 물질
4
실험 절차
A mixture of 1.05 g (6.77 mmol) 3,3,3-trifluoro-2,2-dimethyl-propionamide and 1.48 g (3.66 mmol) Lawesson's reagent in 32 ml dry THF was stirred at reflux temperature for 20 h. After that the reaction mixture was cooled to room temperature and concentrated in vacuo. The residue was purified by chromatography on silicagel (heptane, EtOAc) to afford 0.81 g of the title compound as pure white crystals. MS: M+H=172.
후처리
- temperatureat reflux temperature for 20 h
- concentrationconcentrated in vacuo
- customThe residue was purified by chromatography on silicagel (heptane, EtOAc)
출처 및 근거
- ORD 기록
- ord-df2a498bbddb41b89b5c66f21c6077a4
- 출처 데이터셋
- uspto-grants-2013_01
- 특허 번호
- US08357707B2
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