Nitric Acid → 1-Fluoro-5-methyl-2,4-dinitrobenzene

HRID 73940

반응식

HRID 73940 반응식
[N+]([O-])(O)=O.OS(O)(=O)=O.F[C:11]1C=CC=C(C)C=1.[F:18][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[C:21](C)[C:20]=1[N+:29]([O-:31])=[O:30]>>[F:18][C:19]1[CH:24]=[C:23]([CH3:11])[C:22]([N+:25]([O-:27])=[O:26])=[CH:21][C:20]=1[N+:29]([O-:31])=[O:30]

참가 물질

5

반응물 4

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 9606m-FluorotolueneHCID 137898071-Fluoro-3-methyl-2,4-dinitro-benzene

생성물 1

HCID 5207051-Fluoro-5-methyl-2,4-dinitrobenzene

실험 절차

To a stirred solution of HNO3 (60 mL) and H2SO4 (80 mL), cooled in an ice bath, was added 1-fluoro-3-methyl-benzene (27.5 g, 25 mmol) at such a rate that the temperature did not rise over 35° C. The mixture was allowed to stir for 30 min at room temperature and poured into ice water (500 mL). The resulting precipitate (a mixture of the desired product and 1-fluoro-3-methyl-2,4-dinitro-benzene, approx. 7:3) was collected via filtration and purified by recrystallization from 50 mL isopropyl ether to give 1-fluoro-5-methyl-2,4-dinitro-benzene as a white solid (18 g, 36%).

후처리

  1. customdid not rise over 35° C

출처 및 근거

ORD 기록
ord-864084c6a15d43038ce1102be4fcd1e0
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829204B2

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