HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 2'-O-{2-[(Dimethylamino)oxy]ethyl}-5-methyluridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N,N-Diethylethanamine trihydrofluoride | HCID 175505 | — |
| Reactant | 5'-O-tert-butyldiphenylsilyl-2'-O-[N,N-dimethylaminooxyethyl)-5-methyluridine | HCID 22947701 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2'-O-{2-[(Dimethylamino)oxy]ethyl}-5-methyluridine | HCID 22947699 | 92.5% |
Reaction Steps
Triethylamine trihydrofluoride (3.91 mL, 24.0 mmol) was dissolved in dry THF and triethylamine (1.67 mL, 12 mmol, dry, kept over KOH). This mixture of triethylamine-2HF was then added to 5′-O-tert-butyldiphenylsilyl-2′-O-[N,N-dimethylaminooxyethyl]-5-methyluridine (1.40 g, 2.4 mmol) and stirred at room temperature for 24 hrs. Reaction was monitored by TLC (5% MeOH in CH2Cl2). Solvent was removed under vacuum and the residue placed on a flash column and eluted with 10% MeOH in CH2Cl2 to get 2′-O-(dimethylaminooxyethyl)-5-methyluridine (766 mg, 92.5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06352858B1 |
| Source dataset | uspto-grants-2002_03 |
| ORD ID | ord-eacd02a0b0ef40818bd4b3522b5ce3ff |
| Source note | uspto-grants-2002_03 |