Sulfuric Acid → 3,5-Difluoro-2-nitrobenzonitrile

HRID 1092249

반응식

HRID 1092249 반응식
[N+:1]([O-:4])([O-])=[O:2].[K+].OS(O)(=O)=O.[F:11][C:12]1[CH:13]=[C:14]([CH:17]=[C:18]([F:20])[CH:19]=1)[C:15]#[N:16]>>[F:11][C:12]1[C:13]([N+:1]([O-:4])=[O:2])=[C:14]([CH:17]=[C:18]([F:20])[CH:19]=1)[C:15]#[N:16]

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 24434Potassium NitrateHCID 5872043,5-Difluorobenzonitrile

생성물 1

HCID 545943353,5-Difluoro-2-nitrobenzonitrile수율 95.4%

실험 절차

Potassium nitrate (6.56 g, 64.8 mmol) was added to concentrated H2SO4 (33.7 ml, 633 mmol) at 0° C., followed by slow addition of 3,5-difluorobenzonitrile (4.4 g, 31.6 mmol). The suspension was stirred at this temperature for an additional 3 hours and quenched with ice water (500 ml). The resulting solid was collected by filtration and dried to give the title compound (5.55 g, 95%) as a white solid. 1H NMR (400 MHz, CDCl3) 7.43 (m, 1H), 7.35 (m, 1H).

후처리

  1. customquenched with ice water (500 ml)
  2. filtrationThe resulting solid was collected by filtration
  3. customdried

출처 및 근거

ORD 기록
ord-f555e6cb619a4592bc23723a8bcc8aa1
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129403B2

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