HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 178462815, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 178462817 | HCID 178462817 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178462815 | HCID 178462815 | 74% |
Reaction Steps
A flask is charged with 12.15 g (30.57 mmol) of trans-4-[9-ethyl-6-(4-nitro-phenylamino)-9H-purin-2-yl-amino]-cyclohexanol in 1.15 l of methanol and kept under argon. At 40° C. Raney-Nickel is added slowly, followed by dropwise addition of 15.04 ml (50.06 mmol) of hydrazine monohydrate. After completion the reaction mixture is filtered, the filtrate concentrated and the crude product is purified by chromatography to obtain trans-4-[6-(4-amino-phenyl-amino)-9-ethyl-9H-purin-2-yl-amino]-cyclohexanol (74% yield); ESI-MS: 368 (M+H)+; tRet (HPLC) 7.48 min (method: same system as in method d, gradient 5®40% acetonitrile in 7,5 min.+12 min. 40% acetonitrile).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06767906B2 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-d885b692582d436d90be9390d97f9133 |
| Source note | uspto-grants-2004_07 |