Trifluoroacetic acid → HCID 19047187、化合物
反応式
[CH3:1][C:2]1[CH:3]=[C:4]([S:7][CH2:8][CH:9]=[C:10]([CH3:12])[CH3:11])[S:5][CH:6]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:1][C:2]1[C:3]2[C:10]([CH3:12])([CH3:11])[CH2:9][CH2:8][S:7][C:4]=2[S:5][CH:6]=1参加物
4
実験手順
A solution of 17.36 g (0.088 mol) of the title compound of Step A in 300 mL of methylene chloride was added dropwise to 300 mL of trifluoroacetic acid under nitrogen. After stirring at room temperature overnight, the mixture was evaporated to dryness. The residue was dissolved in 500 mL of methylene chloride, washed with 5% sodium bicarbonate (2×500 mL), dried (MgSO4), filtered, and evaporated to dryness. The crude product was chromatographed on silica gel eluting with hexane to yield 8.26 g of the title compound of Step B as an oil. 1H NMR (CDCl3): δ 1.32 (s,6H), 2.0 (m,2H), 2.3 (s,3H), 3.0 (m,2H), 6.6 (s, 1H).
後処理
- customthe mixture was evaporated to dryness
- dissolutionThe residue was dissolved in 500 mL of methylene chloride
- washwashed with 5% sodium bicarbonate (2×500 mL)
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated to dryness
- customThe crude product was chromatographed on silica gel eluting with hexane
出典と根拠
- ORDレコード
- ord-06dfd4c47a1244c6a03cdd0e38eeceb9
- 出典データセット
- uspto-grants-1997_05
- 特許番号
- US05631210
反応ノート
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