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5,5-Dibromo-4-chloro-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one → 4-chloro-5H,6H,7H-pyrrolo[2,3-d]pyrimidin-6-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5,5-Dibromo-4-chloro-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one | HCID 22390958 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ammonium Chloride | HCID 25517 | — |
| 生成物 | 4-chloro-5H,6H,7H-pyrrolo[2,3-d]pyrimidin-6-one | HCID 12095870 | — |
反応手順
Zinc (6.05 g, 92.56 mmol) was added to a solution of 5,5-dibromo-4-chloro-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one from Step A (3.03 g, 9.26 mmol) in THF (20 mL) and saturated aqueous ammonium chloride (5 mL). After 3 h, the reaction mixture was concentrated in vacuo and purified by HPLC using a reversed phase C18 column and eluting with a gradient of H2O:CH3CN:CF3CO2H-90:10:0.1 to 5:95:0.1. Lyophilization provided the title compound. MS: 71/Z=170 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07696192B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-78aa12f10954491ca32112b36f335302 |
| 出典メモ | uspto-grants-2010_04 |