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Pyridine → 4-[(4-CHLOROPHENYL)METHYL]-6,7-DIHYDRO-2,6-DIMETHYL-3H-IMIDAZO[1,2-a]PURIN-9(4H)-ONE
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Sodium dithionate | HCID 146045 | — |
| 反応物 | 7-amino-8-[(4-chlorophenyl)methyl]-2-methyl-6-nitroso-2,3-dihydroimidazo[1,2-a]pyrimidin-5-one | HCID 178429824 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-[(4-CHLOROPHENYL)METHYL]-6,7-DIHYDRO-2,6-DIMETHYL-3H-IMIDAZO[1,2-a]PURIN-9(4H)-ONE | HCID 178432342 | — |
反応手順
The product of Procedure 99 was reduced with sodium dithionate in formic acid according to the method of Procedure 21. The resulting 7-amino-4-[(4-chlorophenyl)-methyl]-2,3-dihydro-6-formylamino-2-methylimidazo[1,2-a]pyrimidin-5-(8H)-one, 3.5 g. (0.0104 mole) in 7 ml. of pyridine and 7 ml. of acetic anhydride was refluxed for three 3 hrs. during which the mixture foamed and turned dark. The mixture was allowed to cool to room temperature and diluted with acetonitrile resulting in the formation of a white precipitate which was collected. Recrystallized from iPROH/MeOH, yield 800 mg., m.p. 290°-291° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04642345 |
| 出典データセット | uspto-grants-1987_02 |
| ORD ID | ord-3e469c7f6c42491d96434cf4e01bc708 |
| 出典メモ | uspto-grants-1987_02 |