반응 #1135802

반응 방정식

methyl iodide

1-(2-methyl-3-bromophenyl)-1,4-dihydrotetrazole-5-one

N,N-dimethylformamide

sodium hydride

→

1-(2-methyl-3-bromophenyl)-4-methyl-1,4-dihydrotetrazole-5-one

용매

water

반응 조건

후처리

1. 1
   온도cooling
2. 2
   기타To the reaction mixtures
3. 3
   온도cooling
4. 4
   온도The mixtures were raised to room temperature
5. 5
   workup.STIRRINGwere stirred for fourteen hours
6. 6
   기타To the reaction mixtures
7. 7
   추출the mixtures were extracted with ethyl acetate
8. 8
   세척The organic layers were washed with 10% hydrochloric acid, water and saturated saline
9. 9
   건조were dried over anhydrous magnesium sulfate
10. 10
    농축were then concentrated under reduced pressure

실험 절차

To a mixture of the above-mentioned 1-(2-methyl-3-bromophenyl)-1,4-dihydrotetrazole-5-one 31.40 g and N,N-dimethylformamide 250 mL was added 60% sodium hydride 5.90 g under ice-cooling. The mixtures were raised to room temperature and were stirred for one hour. To the reaction mixtures was added methyl iodide 8.4 mL under ice-cooling. The mixtures were raised to room temperature and were stirred for fourteen hours. To the reaction mixtures was added water and the mixtures were extracted with ethyl acetate. The organic layers were washed with 10% hydrochloric acid, water and saturated saline, and were dried over anhydrous magnesium sulfate and were then concentrated under reduced pressure. The resulting residues were subjected to a silica gel column chromatography to give 1-(2-methyl-3-bromophenyl)-4-methyl-1,4-dihydrotetrazole-5-one (hereinafter, referred to as “Intermediate (PRB-P)”) 8.47 g.

출처