HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 66888002, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 4-Methoxybutanoyl chloride | HCID 12794989 | — |
| Reactant | (5-Bromopyridin-2-yl)methanamine | HCID 49761678 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66888002 | HCID 66888002 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
A solution of 9.35 g of C-(5-bromopyridin-2-yl)methylamine [17399-23-0] in 200 ml of ethyl acetate is admixed with 300 ml of saturated aqueous sodium carbonate solution. The reaction mixture is cooled to 0° C. in an ice bath and subsequently admixed dropwise with a solution of 4-methoxybutanoyl chloride [61882-39-1] in 100 ml of ethyl acetate. The reaction mixture is stirred at 0° C. over 1 hour. The phases are separated and the aqueous phase is extracted with 300 ml of ethyl acetate (2×). The combined organic phases are washed with 300 ml of brine, dried over sodium sulphate and concentrated by evaporation. The title compound is identified on the basis of the Rf value from the residue by means of flash chromatography (SiO2 60F).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07868036B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-4871c93f7c6946d5ad8fd09b06bb468a |
| Source note | uspto-grants-2011_01 |