HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → 2-(6-Bromo-pyridin-2-yl)-3-hydroxy-2-hydroxymethyl-propionic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | Ethyl 2-(6-bromopyridin-2-yl)acetate | HCID 53419420 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | 2-(6-Bromo-pyridin-2-yl)-3-hydroxy-2-hydroxymethyl-propionic acid ethyl ester | HCID 86668016 | — |
Reaction Steps
To the solution of para formaldehyde (9.6 g, 319.55 mmol) and sodium ethoxide (0.87 g, 12.784 mmol) in dry THF (250 ml) was added (6-bromo-pyridin-2-yl)-acetic acid ethyl ester (31.2 g, 127.82 mmol) at 0° C. to −10° C. and allowed the reaction mixture to stir at same temperature for 4 h. Solids formed in the reaction mixture were filtered and washed with ethyl acetate and the filtrate was concentrated to obtain crude product as a brown liquid. Yield=30.0 g (crude). TLC (30% ethyl acetate in hexane) Rf=0.28; LCMS: RtH8=0.702, M+1=304.0 and 306.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08637508B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-9aead84618054fb3b907541bf6dd5c19 |
| Source note | uspto-grants-2014_01 |