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Tetrahydrofuran → 4-(N-t-Butoxycarbonyl-N-methylaminomethyl)2,3,4,9-tetrahydrothiopyrano[2,3-b]indole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | O-(1,1-Dimethylethyl) S-(4,6-dimethyl-2-pyrimidinyl) carbonothioate | HCID 148428 | — |
| 反応物 | 4-Methylaminomethyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole | HCID 3056096 | — |
| 生成物 | 4-(N-t-Butoxycarbonyl-N-methylaminomethyl)2,3,4,9-tetrahydrothiopyrano[2,3-b]indole | HCID 20284789 | 93% |
反応手順
To a solution of 4-methylaminomethyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole (4.41 g) in tetrahydrofuran (50 ml) are added triethylamine (4 ml) and 2-(t-butoxycarbonylthio)-4,6-dimethylpyrimidine (4.76 l g) successively at room temperature. The mixture is stirred at room temperature for 2.5 hours and evaporated to remove the solvent. The residue is extracted with chloroform after addition of water. The extract is washed, dried and evaporated to give crude crystals. Recrystallization from acetone gives the title compound (5.57 g) melting at 220°-222° C. (decomp.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04256640 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-769f2ca02fde48049ef46625e6e97232 |
| 出典メモ | uspto-grants-1981_03 |