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

HRID 1092249

反応式

HRID 1092249 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 545943353,5-Difluoro-2-nitrobenzonitrile収率 95.4%

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-f555e6cb619a4592bc23723a8bcc8aa1
出典データセット
uspto-grants-2012_03
特許番号
US08129403B2

関連ノート

読み込み中…