Trifluoroacetic acid → 2-Amino-6,6-dimethylfuro[3,4-d]thiazol-4(6h)-one
反応式
[CH3:1][C:2]1([CH3:19])[C:9]2[S:8][C:7]([NH:10]C(=O)OC(C)(C)C)=[N:6][C:5]=2[C:4](=[O:18])[O:3]1.FC(F)(F)C(O)=O>C(Cl)Cl>[NH2:10][C:7]1[S:8][C:9]2[C:2]([CH3:1])([CH3:19])[O:3][C:4](=[O:18])[C:5]=2[N:6]=1参加物
4
実験手順
To a solution of Example 249A (7.4 g, 26.0 mmol) in CH2Cl2 (20 mL) was added trifluoroacetic acid (20.0 mL, 260 mmol) slowly at 0° C. The reaction mixture was stirred at room temperature for 3 hours, and then concentrated under vacuum. The residue was diluted with ethyl acetate (100 mL) and neutralized with saturated aqueous NaHCO3 solution. The layers were separated and the aqueous phase was extracted with ethyl acetate (5×100 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated to afford the title compound. MS (ESI+) m/z 185 (M+H)+
後処理
- concentrationconcentrated under vacuum
- additionThe residue was diluted with ethyl acetate (100 mL)
- customThe layers were separated
- extractionthe aqueous phase was extracted with ethyl acetate (5×100 mL)
- dry with materialThe combined organic extracts were dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-894236621ac944e185b6475ce2bec794
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841334B2
反応ノート
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