HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 66661918, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 86602288 | HCID 86602288 | — |
| Reactant | HCID 86602290 | HCID 86602290 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66661918 | HCID 66661918 | — |
Reaction Steps
To a solution of 1-(6-azetidin-1-ylpyridin-3-yl)cyclopropanecarbonyl chloride dihydrochloride (64.00 mg, 0.0002067 mol) and (7,7-dimethyl-2-oxobicyclo[2.2.1]hept-1-yl)methanesulfonic acid-(1R)-3H-spiro[furo[3,4-c]pyridine-1,3′-pyrrolidin]-3-one (1:1) (87.3 mg, 0.000207 mol) in methylene chloride (1.00 mL, 0.0156 mol) was added N,N-diisopropylethylamine (0.144 mL, 0.000827 mol) at 0° C. The reaction mixture was stirred at rt for 1-2 h. Upon completion the reaction mixture was diluted with ethyl acetate and washed with water and brine successively, dried with sodium sulfate, filtered, and concentrated. The crude product was purified by prep-LCMS twice to obtain the product as a TFA salt. LCMS: m/z 391.2 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08058288B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-3a634fe89c5f429abc29dd4e4774739a |
| Source note | uspto-grants-2011_11 |