HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl chloroformate → Ammonia
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 66846385 | HCID 66846385 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ammonia | HCID 222 | — |
| Product | HCID 66845304 | HCID 66845304 | — |
Reaction Steps
A solution of (1R)-2-{[6-(2-{[3-(dimethylamino)benzyl]oxy}ethoxy)hexyl]amino}-1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)ethanol (200 mg) in dichloromethane (10 ml) was treated under nitrogen with diisopropylethylamine (0.09 ml) followed by benzyl chloroformate (0.099 ml) and the mixture was stirred at 20° for 4 h. Saturated sodium bicarbonate solution was added and the mixture extracted with dichloromethane. The extract was dried (Na2SO4) and the solvent evaporated in vacuo. The residue was purified by SPE (silica, 10 g). Elution with dichloromethane—ethanol—0.880 ammonia (250:8:1) gave the title compound (220 mg). LCMS RT=3.87 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | USRE044874E1 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-ab38951cd4eb408f9e7fe6dbf197ea31 |
| Source note | uspto-grants-2014_04 |