化工社化工社 化学情報印刷レポート · 研究参考用
2,4-Dichloro-1,3,5-triazine → tert-Butyl 5-(4-chloro-1,3,5-triazin-2-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,4-Dichloro-1,3,5-triazine | HCID 17810 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Tert-butyl octahydropyrrolo(3,4-c)pyrrole-2-carboxylate | HCID 4142526 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ammonium Chloride | HCID 25517 | — |
| 生成物 | tert-Butyl 5-(4-chloro-1,3,5-triazin-2-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate | HCID 86669174 | 44.1% |
反応手順
To a solution of 2,4-dichloro-1,3,5-triazine (150 mg, 0.953 mmol) in ACN (5 mL) was added a solution of Intermediate 15 (202 mg, 0.953 mmol) and DIPEA (0.33 mL, 1.91 mmol) in ACN (5 mL) at 0° C. dropwise. After 10 min the mixture was diluted with saturated aqueous NH4Cl solution. The aqueous layer was then extracted with DCM and the combined organic extracts were dried over Na2SO4, filtered and concentrated in vacuo. Chromatography (Hexanes to 80% EtOAc/Hexanes) afforded the desired product as a white solid (137 mg, 44%). MS (ESI) mass calculated for C14H20ClN5O2, 325.13; m/z found, 326.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653263B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-043734506eae4a778b5a28c884af9189 |
| 出典メモ | uspto-grants-2014_02 |