HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphate → N2-[(3-Iodophenyl)sulfonyl]-N2-{[2-(trimethylsilyl)ethoxy]methyl}glycinamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphate | HCID 1061 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Chloromethyl 2-(trimethylsilyl)ethyl ether | HCID 2724271 | — |
| Reactant | N2-[(3-Iodophenyl)sulfonyl]glycinamide | HCID 21895595 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | N2-[(3-Iodophenyl)sulfonyl]-N2-{[2-(trimethylsilyl)ethoxy]methyl}glycinamide | HCID 69197160 | — |
Reaction Steps
N2-[(3-Iodophenyl)sulfonyl]glycinamide (0.14 g) was stirred with sodium hydride (60% oil dispersion, 0.02 g) in DMF (2 ml) at 21° under nitrogen for 15 min. 2-Trimethylsilylethoxymethyl chloride (0.08 ml) was added and stirring was continued for 1.5 h. The mixture was poured into pH 6.4 phosphate buffer and the product was extracted three times with ethyl acetate. The combined organic layers were washed with brine, dried (MgSO4), concentrated and applied to a silica Bond Elut Cartridge (5 g) in dichloromethane containing methanol. The cartridge was eluted with dichloromethane, diethyl ether and ethyl acetate to give the title compound (0.16 g), LCMS RT=3.49 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07442837B2 |
| Source dataset | uspto-grants-2008_10 |
| ORD ID | ord-9157c2441c4f4a9faa51055c11776a80 |
| Source note | uspto-grants-2008_10 |