1-(4-CHLOROPHENYL)-2-METHOXY-2-OXO-1-ETHANAMINIUM CHLORIDE synthesis
- Product Name:1-(4-CHLOROPHENYL)-2-METHOXY-2-OXO-1-ETHANAMINIUM CHLORIDE
- CAS Number:42718-19-4
- Molecular formula:C9H11Cl2NO2
- Molecular Weight:236.1
67-56-1
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$9.00/25ml
6212-33-5
323 suppliers
$6.00/5g
42718-19-4
53 suppliers
$11.00/100mg
Yield:42718-19-4 100%
Reaction Conditions:
Stage #1: methanolwith thionyl chloride at 0; for 0.75 h;
Stage #2: 2-(4-Chlorophenyl)glycine at 0 - 40; for 48 h;
Steps:
1
Description 1; To ice-chilled methanol (300ml) under argon was carefully added dropwise thionyl chloride (15.44ml; 0.217mol) over 45min. 4-Chlorophenylglycine (26.26g; 0.141 mol) was added, ice cooling removed and the reaction mixture warmed to 400C; the reaction was stirred at 400C for 48h. After cooling to room temperature, the reaction was evaporated under reduced pressure. Re-evaporation from methanol afforded a white solid which was triturated with diethyl ether (ca. 700ml) and then stored at ca. 40C for 64h, filtered, washed with diethyl ether and dried in vacuo to afford the title product as the hydrochloride salt (33.4Og; 100%). 1H NMR (d6-DMSO) δ: 3.72 (3H, s), 5.36 (1 H, s), 7.53 - 7.58 (4H, m), 9.07 (3H, s). Mass Spectrum (Electrospray LC/MS): Found 200 (MH+). C9H1035CINO2 requires 199. Ret. time 1.32 min.
References:
WO2008/92874,2008,A1 Location in patent:Page/Page column 31
6212-33-5
323 suppliers
$6.00/5g
42718-19-4
53 suppliers
$11.00/100mg
104-88-1
630 suppliers
$5.00/25g
42718-19-4
53 suppliers
$11.00/100mg