H-DL-ASP(OME)-OME HCL
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H-DL-ASP(OME)-OME HCL
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CAS No:
14358-33-9
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Formula:
C6H12ClNO4
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Chemical Name:
H-DL-ASP(OME)-OME HCL
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Synonyms:
DL-ASPARTIC ACID DIMETHYL ESTER HYDROCHLORIDE;DL-ASPARTIC ACID(OME)-OME HCL;DL-ASPARTIC ACID ALPHA,BETA-DIMETHYL ESTER HYDROCHLORIDE;H-DL-ASP(OME)-OME HCL;DL-ASPARTIC ACID DIMETHYL ESTERHYDROCHLO RIDE CRYST;dl-asparticaciddimethylesterHCl;DL-Asp(OMe)-OMe·HCl;DL-ASPARTIC ACID A,B-DIMETHYLESTER HYDROCHLORIDE
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CAS No:
H-DL-ASP(OME)-OME HCL Use and Manufacturing
To the reaction vessel was added 106.8 g (0.8 mol) of D-aspartic acidAnd 700 ml of methanol, 84.4 ml (1.2 mol) of thionyl chloride was slowly added with stirring, The reaction temperature was controlled at 0 ° C, After the addition of thionyl chloride, Stirring was continued at room temperature at 29 deg.] C, After 30 hours of reaction, The reaction solution was distilled off to remove excess methanol and thionyl chloride, The remaining oil was crystallized from 3.5 times the ether, Get the white crystal, filter, Washed three times with ether, Dried to give 107.8 g of white solid D-aspartic acid dimethyl ester hydrochloride;General procedure: Under ice cooling, chlorotrimethylsilane (33.2ml, 263.0mmol) was added dropwise to a suspension of (S)-aspartate (10g, 75.1mmol, 98percent ee) in methanol abs. (150ml) and the reaction mixture was stirred for 16h at room temperature. The solvent and volatile byproducts were evaporated in vacuo. The residue was suspended in methanol (1×30ml) and the solvent was removed in vacuo. Then diethyl ether was added (30ml) and the solvent was removed under reduced pressure. This procedure was repeated three times. The product was dried in high-vacuum. Colorless solid, mp 112–115°C, yield 15g (100percent).
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