HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzylamine → HCID 56953824, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzylamine | HCID 7504 | — |
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | HCID 86691065 | HCID 86691065 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 56953824 | HCID 56953824 | — |
Reaction Steps
To a solution of (D1) (20 g, 0.125 mol) in CH2Cl2 (300 ml, 15 vol) and tetrahydrofuran (THF) (100 ml, 5 vol), N-methylmorpholine (NMM) (16.6 ml, 0.15 mol) was added slowly at −40° C. After 20 min, isobutylchloroformate (IBCF) (19.67 ml, 0.15 mol) was added at same temperature and stirred for 20 min. Benzylamine (16.5 ml, 0.15 mol) in tetrahydrofuran (40 ml) was added at −40° C., then the reaction mixture was stirred for 1 h and allowed to room temperature. Solvent was evaporated under reduced pressure. The obtained crude was purified by column chromatography in 5% methanol in chloroform to afford (A1) as a white colored powder. Yield: 17 g; 55%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08969620B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-972720d7d0b546e2acf6ef226f9ecda0 |
| Source note | uspto-grants-2015_03 |