Phosphorus sulfide (P2S5) → HCID 21836471、化合物
反応式
[F:1][C:2](=[C:13]([F:15])[F:14])[CH2:3][C:4]([NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=O.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:17]>C1COCC1>[F:1][C:2](=[C:13]([F:15])[F:14])[CH2:3][C:4](=[S:17])[NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1参加物
4
実験手順
A mixture of 3,4,4-trifluoro-N-phenyl-3-butenamide (1.0 g, 4.65 mmol) end phosphorus pentasulfide (2.07 g, 4.65 mmol) in anhyd. THF (100 mL) was heated at reflux under nitrogen for 1 hour. The reaction mixture was cooled to r.t. and filtered. The filtrate was concentrated and the residue was chromatographed over silica gel (dichloromethane/hexanes, 80/20) to give 0.65 g (60%) of the desired compound as a pale yellow solid. m.p. 65°-67° C.
後処理
- temperatureat reflux under nitrogen for 1 hour
- filtrationfiltered
- concentrationThe filtrate was concentrated
- customthe residue was chromatographed over silica gel (dichloromethane/hexanes, 80/20)
出典と根拠
- ORDレコード
- ord-10b5e6be58ad4131a74f5672591cff0b
- 出典データセット
- uspto-grants-1997_05
- 特許番号
- US05627174
反応ノート
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