반응 #67952

반응 방정식

sodium triacetoxyborohydride

tert-butyl 4-amino-4-methylpiperidine-1-carboxylate

2,3-dihydro-1,4-benzodioxin-6-carbaldehyde

sodium hydrogen carbonate

sodium triacetoxyborohydride

→

tert-butyl 4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)-4-methylpiperidine-1-carboxylate

용매

chloroform

acetic acid

dichloromethane

반응 조건

후처리

1. 1
   workup.ADDITIONwere added
2. 2
   workup.STIRRINGstirred at the same temperature for 30 minutes
3. 3
   workup.STIRRINGstirred at the same temperature for 30 minutes
4. 4
   workup.STIRRINGthe reaction mixture was stirred for 1 hour
5. 5
   온도under reflux
6. 6
   온도by heating
7. 7
   기타The organic layer was separated
8. 8
   추출the aqueous layer was extracted with chloroform
9. 9
   세척the resultant solution was washed with an aqueous saturated sodium chloride solution
10. 10
    건조dried over anhydrous magnesium sulfate
11. 11
    기타the solvent was removed under reduced pressure

실험 절차

To 5 mL of a dichloromethane solution containing 0.50 g of tert-butyl 4-amino-4-methylpiperidine-1-carboxylate, 0.38 g of 2,3-dihydro-1,4-benzodioxin-6-carbaldehyde and 0.13 mL of acetic acid were added, and the mixture was stirred at room temperature for 3 hours. The reaction mixture was added with 0.74 g of sodium triacetoxyborohydride and stirred at the same temperature for 30 minutes. The reaction mixture was added with 0.74 g of sodium triacetoxyborohydride and stirred at the same temperature for 30 minutes, and then the reaction mixture was stirred for 1 hour under reflux by heating. Thereto were added chloroform and an aqueous saturated sodium hydrogen carbonate solution. The organic layer was separated, and the aqueous layer was extracted with chloroform. The organic layer and the extract were combined, and the resultant solution was washed with an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 0.81 g of a light brown oily substance, tert-butyl 4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)-4-methylpiperidine-1-carboxylate.

출처