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N-bromobutanimide → 7-Bromo-2-chloro-5H-pyrrolo[3,2-d]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 2-Chloro-5H-pyrrolo[3,2-d]pyrimidine | HCID 45789986 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 7-Bromo-2-chloro-5H-pyrrolo[3,2-d]pyrimidine | HCID 86731161 | 75.3% |
反応手順
A solution of 2-chloro-5H-pyrrolo[3,2-d]pyrimidine (1.54 g, 10 mmol) in DMF (10 mL) was added NBS (2.00 g, 11 mmol) at room temperature. The resulting solution was stirred for 1 h and diluted with EtOAc. The resulting solution was washed with a sat. aq. solution of NaHCO3, H2O and brine. The EtOAc layer was dried (Na2SO4), concentrated and purified by ISCO to provide the desired product (1.75 g, 75%). 1H NMR (400 MHz, CD3OD) δ 8.53 (s, 1H), 7.60 (s, 1H); MS m/z 234.0 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09273056B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-15074791c24c4f36aac2fea6e8b49469 |
| 出典メモ | uspto-grants-2016_03 |