2-Hydroxyethyl acrylate → HCID 178460505, compound
Reaction equation
[OH:1][C:2]1[N:7]2[N:8]=[CH:9][N:10]=[C:6]2[N:5]=[C:4]([CH2:11][C:12]([OH:14])=[O:13])[CH:3]=1.O[CH2:16][CH2:17][O:18][C:19](=[O:22])[CH:20]=[CH2:21]>CN(C)C=O>[C:19]([O:18][CH2:17][CH2:16][O:13][C:12]([CH2:11][C:4]1[CH:3]=[C:2]([OH:1])[N:7]2[N:8]=[CH:9][N:10]=[C:6]2[N:5]=1)=[O:14])(=[O:22])[CH:20]=[CH2:21]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
19.4 g of 7-hydroxy-5-carboxymethyl-1,2,4-triazolo[1,5-a]pyrimidine and 12 g of hydroxyethylacrylate were dissolved in 150 ml of dimethylformamide (DMF) and thereto, a solution of 20.6 g of N,N-dicyclohexylcarbodiimide in 30 ml of DMF was added dropwise at a room temperature for 10 minutes. Thereafter, stirring was continued at a room temperature for 8 hours, and the precipitate produced was removed by filtration. The filtrate was condensed under a reduced pressure and low temperature. The thus obtained residue was chromatographed through silica gel put in a column in order to separate it into components and purify. The intended compound was obtained in a form of crystal. It was recrystallized from ethyl acetate. Thus, 6 g of white crystal having a melting point of 108° to 109° C. (intended compound) was obtained.
Workup
- customthe precipitate produced
- customwas removed by filtration
- customcondensed under a reduced pressure and low temperature
- customThe thus obtained residue was chromatographed through silica gel
- customto separate it into components
- custompurify
- customThe intended compound was obtained in a form of crystal
- customIt was recrystallized from ethyl acetate
- customwas obtained
Sources & evidence
- ORD record
- ord-7409ad4aeed5444f89a83aa8822a0210
- Source dataset
- uspto-grants-1983_08
- Patent number
- US04397943
Reaction notes
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