Nitric Acid → 2,6-Difluoro-3-nitrotoluene

HRID 1098549노트

반응식

HRID 1098549 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[CH3:9].[N+:10]([O-])([OH:12])=[O:11]>OS(O)(=O)=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N+:10]([O-:12])=[O:11])=[C:4]([F:8])[C:3]=1[CH3:9]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 5814931,3-Difluoro-2-methylbenzene

생성물 1

HCID 127954862,6-Difluoro-3-nitrotoluene수율 78%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A solution of 1,3-difluoro-2-methyl-benzene (15 g, 0.12 mol) in conc. H2SO4 (100 mL) was treated drop wise with 65% HNO3 (11.4 g, 0.12 mol) at −10° C. and the resultant mixture was stirred for about 30 min. The mixture was poured into ice-water and extracted with ethyl acetate (3×200 mL). The combined organic layers were washed with brine, dried (Na2SO4) and concentrated in vacuo to give 1,3-difluoro-2-methyl-4-nitro-benzene (16 g, 78% yield) 1H NMR (400 MHz, CDCl3): δ 7.80 (m, 1 H), 6.95 (m, 1H), 2.30 (s, 3 H).

후처리

  1. extractionextracted with ethyl acetate (3×200 mL)
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-93701d2877e14a249fa2a6eb11d2943c
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143293B2

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