반응 #67498

반응 방정식

2-bromo-1-difluoromethoxy-3-nitro-benzene

CuCN

LiBr

→

2-difluoromethoxy-6-nitrobenzonitrile

수율 84.6%

용매

tetrahydrofuran

toluene

반응 조건

후처리

1. 1
   온도The reaction mixture is cooled to ambient temperature
2. 2
   세척washed with aqueous sodium bromide (1M) and aqueous sodium hydrogen sulfite (saturated)
3. 3
   건조The organic phase is dried over sodium sulfate
4. 4
   농축concentrated
5. 5
   기타The residue is purified by HPLC

실험 절차

A mixture of 2-bromo-1-difluoromethoxy-3-nitro-benzene (1 g, 3.7 mmol), CuCN (0.40 g, 4.5 mmol) and LiBr (0.32 g, 3.7 mmol) in tetrahydrofuran (10 ml) are heated in a microwave oven at 200° C. for 40 minutes. The reaction mixture is cooled to ambient temperature, diluted with toluene and washed with aqueous sodium bromide (1M) and aqueous sodium hydrogen sulfite (saturated). The organic phase is dried over sodium sulfate and concentrated. The residue is purified by HPLC to give 2-difluoromethoxy-6-nitrobenzonitrile (0.67 g, 84% yield). 1H-NMR (CDCl3, 400 MHz): 8.20 (d, 1H), 7.85 (t, 1H), 7.75 (d, 1H), 6.75 (t, 1H) ppm.

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