関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl 1-(6-amino-9-((2R,3R,4S,5R)-3,4-dihydroxy-5-(hydroxymethyl)tetrahydrofuran-2-yl)-9H-purin-2-yl)-1H-pyrazole-4-carboxylate | HCID 9865974 | — |
| 反応物 | 2-Hydrazinoadenosine | HCID 10357262 | — |
| 反応物 | Ethyl 2-formyl-3-oxopropanoate | HCID 11029955 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178472218 | HCID 178472218 | — |
反応手順
A reaction vessel is charged with 2-hydrazinoadenosine (450 g) and absolute ethanol (11376 g). HCl (7.47 g) and ethyl 2-formyl-3-oxopropionate (1557 g) are added. The mixture is heated to reflux and sampled until the level of residual 2-hydrazinoadenosine in the mixture is not more than 0.50% and the level of the compound of formula (3) is not more than 2.5%. The mixture is slowly cooled to approximately 10° C. The product, the compound of formula (4) is isolated by filtration and washed with absolute ethanol (5121 g). The product is dried under vacuum at up to 40° C. until residual ethanol is not more than 5000 ppm to give ethyl (2E)-3-({9-[(4S,2R,3R,5R)-3,4-dihydroxy-5-(hydroxymethyl)oxolan-2-yl]-2-[4-(ethoxycarbonyl)-pyrazolyl]purin-6-yl}amino)-2-formylprop-2-enoate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07956179B2 |
|---|
| 出典データセット | uspto-grants-2011_06 |
|---|
| ORD ID | ord-f62910ef1f7b481fbcc4b5ccd04812f4 |
|---|
| 出典メモ | uspto-grants-2011_06 |
|---|
