반응 #1118669

반응 방정식

2-bromo-3-methoxy pyridine

(1S,4S)-N-benzyl-2,5-diazabicyclo[2.2.1]heptane

→

desired product

수율 51.0%

2-(3-methoxy-2-pyridinyl)-5-phenylmethyl-(1S,4S)-2,5-diazabicyclo[2.2.1]-heptane

수율 51.0%

용매

CH2Cl2

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled to 23° C.
2. 2
   추출extracted with 5% NaHCO3, and finally wit
3. 3
   건조The organic layer was dried over K2CO3
4. 4
   여과filtered
5. 5
   농축concentrated under reduced pressure
6. 6
   기타The crude oil was purified by silica gel chromatography (CH2Cl2 :MeOH; 96:4)

실험 절차

A mixture of 2-bromo-3-methoxy pyridine (9.9 g) and (1S,4S)-N-benzyl-2,5-diazabicyclo[2.2.1]heptane (10.9 g) was heated at 100° C. in a Parr bomb for 67 h. The reaction mixture was cooled to 23° C., dissolved in CH2Cl2, extracted with 5% NaHCO3, and finally wit:h H2O. The organic layer was dried over K2CO3, filtered, and concentrated under reduced pressure. The crude oil was purified by silica gel chromatography (CH2Cl2 :MeOH; 96:4) to give the desired product (7.93 g, 51%).

출처