HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1434655-18-1
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | tert-Butyl 2-methylalaninate | HCID 7019940 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1434655-18-1 | HCID 89557264 | 298.8% |
Reaction Steps
Into a 100-mL 3-necked round-bottom flask was placed a solution of tert-butyl 2-amino-2-methylpropanoate (1.2 g, 7.54 mmol, 1.00 equiv) in dichloromethane (20 mL). This was followed by the addition of ditrichloromethyl carbonate (750 mg, 2.53 mmol, 0.34 equiv), in portions at 0° C. After 30 min, triethylamine (2.3 g, 22.73 mmol, 3.02 equiv) was added dropwise with stirring. The resulting solution was stirred for 5 h at room temperature and then concentrated under vacuum. The residue was diluted with 20 mL of ethyl ether. The solids were filtered out. The filtrate was concentrated under vacuum. Purification afforded 1.4 g (crude) of tert-butyl 2-isocyanato-2-methylpropanoate (110.2) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08969557B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-8686c9ac0d65419fab27d6b5750e4036 |
| Source note | uspto-grants-2015_03 |