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Dimethylformamide → (1-(7-Benzyl-1,3-dimethyl-2,6-dioxo-1,2,3,6-tetrahydropurin-8-yl)pyrrolidin-3-yl)carbamic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 7-Benzyl-8-chloro-1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione | HCID 325372 | — |
| 反応物 | (3S)-(-)-3-(tert-Butoxycarbonylamino)pyrrolidine | HCID 1514396 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | (1-(7-Benzyl-1,3-dimethyl-2,6-dioxo-1,2,3,6-tetrahydropurin-8-yl)pyrrolidin-3-yl)carbamic acid tert-butyl ester | HCID 69136344 | — |
反応手順
7-Benzyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione (2A) (100 mg, 0.33 mmol), (3S)-(−)-3-(tert-butoxycarbonylamino)pyrrolidine (305 mg, 1.64 mmol), and triethylamine (0.46 ml, 3.28 mmol) was dissolved in 20 ml of 2-propanol and 5 ml of DMF and the mixture was subjected to microwaves (method F, 130° C., 300 W) for three hours. The solvent was evaporated and the crude product was purified by preparative HPLC (method A1, Rt=11.75 min.). Evaporation of the solvent afforded compound (3A) as a brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07192952B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-ab4c48330f244552b739e231d2105881 |
| 出典メモ | uspto-grants-2007_03 |