HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl Bromide → HCID 66712473, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl Bromide | HCID 6323 | — |
| Reactant | HCID 66712386 | HCID 66712386 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 66712473 | HCID 66712473 | — |
Reaction Steps
To (1R,2S)-2-((R)-2′-cyclopentyl-2′-hydroxy 2′-phenylacetoxy)-7-methyl-7-azabicyclo[2.2.1]heptane (46 mg, 0.139 mmol) in acetone (2 mL) was added 1 mL of methyl bromide solution (2M in ether). The resulting mixture was left at room temperature for 48 hrs. The crystallized product was filtered off and dried to yield 36 mg of (1R,2S)-2-((R)-2′-cyclopentyl-2′-hydroxy 2′-phenylacetoxy)-7,7-dimethyl-7-azoniabicyclo[2.2.1]heptane bromide (2) as a white crystalline solid, M.P. 233-234° C., 1HNMR: 7.6 (dd, 2H); 7.4 (m, 2H); 7.28 (m, 1H); 5.0 (m, 1H); 4.9 (m, 1H); 4.45 (m, 1H); 3.8 (s, 1H); 3.49 (s, 3H); 3.28 (s, 3H); 3.0 (m, 1H); 2.5-2.2 (m, 4H); 1.9-1.3 (m, 10H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09320731B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-a4017aaa890e42f2bc5b3bc413ef3144 |
| Source note | uspto-grants-2016_04 |