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Triethylamine → 4,4,6,6-Tetramethyl-4,6-dihydrofuro[3,4-d]thiazol-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 反応物 | 4-Bromo-2,2,5,5-tetramethyldihydrofuran-3(2h)-one | HCID 12201745 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4,4,6,6-Tetramethyl-4,6-dihydrofuro[3,4-d]thiazol-2-amine | HCID 79006302 | — |
反応手順
To a solution of Example 248A (10.0 g, 0.045 mol) in ethanol (100 mL) were added thiourea (3.8 g, 0.05 mol) and triethylamine (6.3 mL, 0.045 mol). The reaction mixture was heated at reflux overnight, then cooled, and concentrated under reduced pressure. The residue was diluted with water (25 mL) and extracted with ethyl acetate (3×50 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated. The residue was purified by column chromatography (SiO2, 0-5% methanol in CH2Cl2) to afford the title compound MS (ESI+) m/z 199 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08546583B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-e32efb3469c84a7089ed7ef148b91642 |
| 出典メモ | uspto-grants-2013_10 |