関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Amino-1-dimethylaminopropane | HCID 99027 | — |
| 反応物 | 5-Amino-6-nitro-1H-isoindole-1,3(2H)-dione | HCID 15144568 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 66793432 | HCID 66793432 | 64% |
反応手順
A mixture of 5-amino-6-nitro-isoindole-1,3-dione (1.66 g, 8.0 mmol), HCl salt of 2-amino-N,N-dimethyl-propylamine (5.3 g, crude, <30 mmol), imidazole (1.36 g, 20 mmol) and Et3N (8.4 mL, 6.07 g, 60 mmol) in dioxane (80 mL) was sealed in a ChemGlass heavy wall pressure flask. After it was heated at 130° C. for 72 h, the reaction mixture was evaporated to dryness at 95° C. (the bath temperature) under reduced pressure. The chromatography of the residue with CH2Cl2/MeOH/28% aqueous NH4OH (240:10:1) afforded the title compound (1.49 g, 64%). 1H NMR (DMSO-d6) δ 1.32 (d, J=6 Hz, 3H, CH3), 2.09 (s, 6H, 2CH3), 2.25 (m, 1H), 2.95 (m, 1H), 4.35 (m, 1H), 7.43 (s, 1H), 8.29 (s, 1H), 8.39 (br s, 2H, NH). ESI-MS m/z 293.1 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08063225B2 |
|---|
| 出典データセット | uspto-grants-2011_11 |
|---|
| ORD ID | ord-05296fc8dc2647c29d34d863fda2fccf |
|---|
| 出典メモ | uspto-grants-2011_11 |
|---|
