HuagongsheHuagongshe Chemistry Print Report · For research reference only
N,N-Diethylethanamine trihydrofluoride → 3'-Deoxy-3'-(iodomethyl)-2'-O-(2-methoxyethyl)-5-methyluridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N,N-Diethylethanamine trihydrofluoride | HCID 175505 | — |
| Reactant | 5'-O-(tert-butyldiphenylsilyl)-3'-deoxy-3'-(iodomethyl)-2'-O-(2-methoxyethyl)-5-methyluridine | HCID 23518341 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3'-Deoxy-3'-(iodomethyl)-2'-O-(2-methoxyethyl)-5-methyluridine | HCID 23518331 | 69.4% |
Reaction Steps
A solution of 5′-O-(tert-butyldiphenylsilyl)-3′-deoxy-3′-(iodomethyl)-2′-O-(2-methoxyethyl)-5-methyluridine (1.12 g, 1.65 mmol) and triethylamine trihydrofluoride (1.1 mL, 1.1 g, 6.7 mmol) in 20 mL of THF was stirred at rt for 24 h. The reaction mixture was diluted with 50 mL of ethyl acetate and washed with water and brine. The organic phase was dried (Na2SO4) and concentrated. The residue was purified by flash chromatography on a silica gel column. Gradient elution with 2:1, 1:2 and then 1:3 hexanes-EtOAc provided 504 mg of the title compound as a white foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07202224B2 |
| Source dataset | uspto-grants-2007_04 |
| ORD ID | ord-e2db42fe3984474fb43787c3ebc60974 |
| Source note | uspto-grants-2007_04 |