HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 67148364, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 67148302 | HCID 67148302 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67148364 | HCID 67148364 | 45.2% |
Reaction Steps
To a sol. of {3-[(tert-butoxycarbonyl-cyclopropyl-amino)-methyl]-4-chloro-phenyl}-acetic acid (4.30 g, 12.6 mmol) in CH2Cl2 (130 mL) was added 1-chloro-N,N-2-trimethylpropenyl amine (1.87 mL, 15.2 mmol), and the mixture was stirred for 60 min. Methylamine (2M in THF, 25.0 mL, 50.0 mmol) was added, and the mixture was stirred overnight. More CH2Cl2 was added, and the mixture was washed with water and brine, was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the crude by FC (EtOAc/heptane 7:3) yielded the title compound (2.01 g, 45%). LC-MS: tR=0.95 min; ES+: 325.30.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07968720B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-ac05a9a6630a47b18cbb4f7515b2f90d |
| Source note | uspto-grants-2011_06 |