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Sodium dithionate → 4-[(4-CHLOROPHENYL)METHYL]-6,7-DIHYDRO-6-METHYL-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 | Sodium dithionate | HCID 146045 | — |
| 反応物 | 7-amino-8-[(4-chlorophenyl)methyl]-2,3-dihydro-6-formylamino-2-methylimidazo-[1,2-a]pyrimidin-5(8H)-one | HCID 12683839 | — |
| 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 | — |
| 生成物 | 4-[(4-CHLOROPHENYL)METHYL]-6,7-DIHYDRO-6-METHYL-3H-IMIDAZO[1,2-a]PURIN-9(4H)-ONE | HCID 178429822 | — |
反応手順
The nitroso compound of Procedure 99 was reduced with sodium dithionate in formic acid according to the method of Procedure 21. The resulting 7-amino-8-[(4-chlorophenyl)methyl]-2,3-dihydro-6-formylamino-2-methylimidazo[1,2-a]pyrimidin-5(8H)-one, 185 g., (0.54 mole) was then dissolved with heating in 1 l. of 0.6N NaOH, the solution clarified by filtration, the filtrate acidified with acetic acid, and allowed to cool resulting in precipitation of the desired product, yield 71.7 g., recrystallized from ethylene glycol monomethyl ether/(iPr)2O, m.p. 259°-260.5°.
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-7aa0639b5c5b47c4bb4fb29ab4951474 |
| 出典メモ | uspto-grants-1987_02 |