HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → HCID 86647439, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | (2,6-Dichloropyridin-4-yl)methanol | HCID 2794840 | — |
| Product | HCID 86647439 | HCID 86647439 | — |
Reaction Steps
A mixture of crude (2,6-dichloropyridin-4-yl)methanol in 7 mL of (CH3)2NH (40 wt % solution in H2O) was stirred at r.t. for 45 min. The temperature was increased to 50° C., and the solution was stirred at 50° C. for about 24 h. Ethyl acetate and H2O (15 mL) were added, and the aqueous layer was extracted with EtOAc. The combined extracts were washed with brine, and the aqueous layer was extracted with EtOAc. The combined extracts were dried over Na2SO4, filtered, and concentrated. Purification by flash silica gel chromatography (40% EtOAc/hexanes) provided 1.01 g of (2-chloro-6-(dimethylamino)pyridin-4-yl)methanol with some impurity (unreacted starting material).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08299267B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-8f2286edbd2c4ac6b3e12b4ef8bd506d |
| Source note | uspto-grants-2012_10 |