Lawesson's reagent → 3,3,3-Trifluoro-2,2-dimethyl-thiopropionamide
反応式
[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]参加物
4
実験手順
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.
後処理
- temperatureat reflux temperature for 20 h
- concentrationconcentrated in vacuo
- customThe residue was purified by chromatography on silicagel (heptane, EtOAc)
出典と根拠
- ORDレコード
- ord-df2a498bbddb41b89b5c66f21c6077a4
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08357707B2
反応ノート
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