HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 22987252, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 1,1-Dichloroethane | HCID 6365 | — |
| Reactant | Trimethylacetamide | HCID 12957 | — |
| Reactant | L-Serine, methyl ester, hydrochloride (1:1) | HCID 2723730 | — |
| Reactant | Triethyloxonium tetrafluoroborate | HCID 2723982 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22987252 | HCID 22987252 | — |
Reaction Steps
3 g (29.6 mmol) of pivalic acid amide are stirred with 5.6 g (29.6 mmol) of triethyloxonium tetrafluoroborate in 50 ml of dichloromethane for 48 h. Ammonia is passed through the solution over a period of 3 h, the resulting residue is filtered off and the filtrate is concentrated in a rotary evaporator. 4.67 g (30 mmol) of L-serine methyl ester hydrochloride are added with 50 ml of dichloroethane, and the mixture is then heated at reflux for 8 h. Extraction with NaHCO3 solution and NH4Cl solution, drying over MgSO4 and purification by column chromatography (15×3 cm, pentane/diethyl ether 4:1) are carried out. Yield 1.34 g (24% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06498256B2 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-2a45592384054758a470d9b4218c5735 |
| Source note | uspto-grants-2002_12 |