반응 #502107

반응 방정식

water

ammonium chloride

N-methoxy-N-methyl-1H-indazole-3-carboxamide

methylmagnesium bromide

→

compound

1-(1H-Indazol-3-yl)ethanone

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도It is cooled to 0° C.
2. 2
   추출The mixture is extracted with 40 ml of ethyl acetate
3. 3
   세척The organic phase is washed with 40 ml of a saturated solution of sodium chloride
4. 4
   건조dried over magnesium sulphate
5. 5
   농축concentrated under reduced pressure
6. 6
   기타The residue is purified by silica gel chromatography, elution

실험 절차

In a round-bottomed flask, 2.4 g of N-methoxy-N-methyl-1H-indazole-3-carboxamide are placed in 140 ml of tetrahydrofuran at 0° C. and under argon. 19 ml of methylmagnesium bromide (3M in ethyl ether) are added dropwise. The mixture is stirred for one hour at 0° C. and 20 h at ambient temperature. It is cooled to 0° C. and 80 ml of water and 40 ml of a saturated solution of ammonium chloride are added. The mixture is extracted with 40 ml of ethyl acetate. The organic phase is washed with 40 ml of a saturated solution of sodium chloride, dried over magnesium sulphate and then concentrated under reduced pressure. The residue is purified by silica gel chromatography, elution being carried out with a heptane/ethyl acetate mixture. 1.6 g of compound are obtained.

출처