1,1-Dichlorodimethyl ether synthesis
- Product Name:1,1-Dichlorodimethyl ether
- CAS Number:4885-02-3
- Molecular formula:C2H4Cl2O
- Molecular Weight:114.96
79-37-8
482 suppliers
$17.67/10gm:
107-31-3
354 suppliers
$16.00/25mL
4885-02-3
194 suppliers
$10.00/1g
Yield:4885-02-3 71%
Reaction Conditions:
with N-methyl-N-phenylformamide at 25 - 30; for 31 h;
Steps:
Method A
Oxalyl chloride 127 g (1 mol) was slowly added dropwise to a mixture of methyl formate 90 g (1.5 mol) and N-methylformanilide 13.5 g (0.1 mol) at 25-30 °C for 7 h. (the condenser was cooled with ice-water) The mixture was stirred for a further 24 h at the same temperature until generation of the gas had stopped. The mixture was distilled through a 300 mm vigreux column to give 81.4 g of 2a (71% yield) having bp 83-84 °C (lit 6a 82-85.5 °C). GCMS: m/z = 79 (M-35, base peak): 81 (M-35+2) = 3:1. 1H NMR (300 MHz, CDCl3): δ 3.68 (s, 3H, CH3), 7.34 (s, 1H, CH). 13C NMR (75 MHz, CDCl3): δ 52.56, 98.82.
References:
Kimura, Yoshikazu;Warashina, Takuya [Tetrahedron Letters,2017,vol. 58,# 49,p. 4598 - 4599]
107-31-3
354 suppliers
$16.00/25mL
4885-02-3
194 suppliers
$10.00/1g
