TERT-BUTYL 4-(DIBROMOMETHYLENE)PIPERIDINE-1-CARBOXYLATE synthesis
- Product Name:TERT-BUTYL 4-(DIBROMOMETHYLENE)PIPERIDINE-1-CARBOXYLATE
- CAS Number:305794-65-4
- Molecular formula:C11H17Br2NO2
- Molecular Weight:355.07
Yield:305794-65-4 100%
Reaction Conditions:
with triphenylphosphine in dichloromethane at 0 - 20; for 72 h;Inert atmosphere;
Steps:
2.27.a Step a Intermediate 19 tert- ut ] 4-(dibromomethylidene)piperidine-l-carboxylate
Step a Intermediate 19 tert- ut ] 4-(dibromomethylidene)piperidine-l-carboxylate A solution of tert-butyl 4-oxopiperidine-l -carboxylate (30 g, 151 mmol) and triphenylphosphme (79 g, 301 mmol) in DCM (300 ml) cooled to 0°C under nitrogen was treated portionwise with carbon tetrabromide (100 g, 301 mmol) and stirred at 0° C for 3 h before allowing to warm to r.t. and stining for 3 days. The reaction mixture was filtered and the filtrate evaporated to dryness. Et20 was added, the mixture stirred for 1 h and filtered. The filtrate was concentrated to give tert-butyl 4- (dibromomethylidene)piperidine-l-carboxylate contaminated with triphenylphosphine oxide as a white solid (53.9 g, quantitative). ? NMR (400 MHz, DMSO-
References:
WO2013/27001,2013,A1 Location in patent:Page/Page column 61
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