ETHYL 3,4-DICHLORO-5-METHYL-1H-PYRROLE-2-CARBOXYLATE synthesis
- Product Name:ETHYL 3,4-DICHLORO-5-METHYL-1H-PYRROLE-2-CARBOXYLATE
- CAS Number:24691-21-2
- Molecular formula:C8H9Cl2NO2
- Molecular Weight:222.07
3284-51-3
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Yield:24691-21-2 77%
Reaction Conditions:
with sulfuryl dichloride in Carbon tetrachloride at 0; for 1 h;
Steps:
Intermediate 29; Ethyl 3 ^-dichloro-S-methyl- l/j-pyrrole-2-carboxylate; A solution of ethyl 5 -methyl- li/-pyrrole-2-carboxy late (Intermediate 30; 7.00 g, 0.0457 mol) in tetrachloromethane (30 ml) was cooled to 0 °C under nitrogen. The rubber10 septum used in the apparatus was pierced with a needle, and SO2Cl2 (7.8 ml, 0.096 mol) was then added dropwise over 25 minutes. Within 1 hr, the reaction mixture had formed a slurry. The solid was collected by suction filtration, washed with cold tetrachloromethane, and dried under vacuum overnight to give the title product as a peach coloured solid (7.84 g, 0.0353 mol, 77% yield). NMR: 1.34-1.40 (t, 3H), 2.28 (s, 3H), 4.32-4.38 (m, 2H); MS (ES"): 222.00,15 224.00 (M-H)" for C8H9Cl2NO2.
References:
WO2006/87548,2006,A2 Location in patent:Page/Page column 59
24691-22-3
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636-41-9
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