참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 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 | — |
| 반응물 | 2-Hydrazinoadenosine | HCID 10357262 | — |
| 반응물 | Ethyl 2-formyl-3-oxopropanoate | HCID 11029955 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 178472218 | HCID 178472218 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07671192B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_03 |
|---|
| ORD ID | ord-3d29700967b14b699c0cf98ca0cb5e0f |
|---|
| 출처 메모 | uspto-grants-2010_03 |
|---|
