化工社化工社 化学情報印刷レポート · 研究参考用
1,8-Diazabicyclo(5.4.0)undec-7-ene → 5-tert-Butyl-3-(2-chloro-benzyl)-7-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | 1,3-Propanesultam | HCID 642157 | — |
| 反応物 | 5-tert-butyl-7-chloro-3-(2-chlorobenzyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine | HCID 86683284 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-tert-Butyl-3-(2-chloro-benzyl)-7-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine | HCID 86683290 | 16% |
反応手順
A mixture of 5-tert-butyl-7-chloro-3-(2-chlorobenzyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine (15.9 mg, 47.2 μmol), 1,1-dioxo-isothiazolidine (11.4 mg, 94.4 μmol) and DBU (14.2 μL, 94.4 μmol) in DMF (250 μL) was stirred at the room temperature overnight. The reaction mixture was directly purified by preparative HPLC (column: Gemini Sum C18 110A 75×30 mm. mobile phase: water (0.05% Et3N): acetonitrile 75:25% to 5:95%. WL: 230 nm Flow: 30 mL/min.) to afford the title compound as white solid (3.10 mg, 16%). MS (m/e): 387.3 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08741906B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-80588c1206c5471db8ded5e80daec0fa |
| 出典メモ | uspto-grants-2014_06 |