Sulfuric Acid → N-(3-Nitro-2,4-dimethyl-benzyl)-2,2,2-trifluoroacetamide

HRID 2042798ノート

反応式

HRID 2042798 の反応式
O[CH2:2][NH:3][C:4](=[O:9])[C:5]([F:8])([F:7])[F:6].[CH3:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[C:12]=1[N+:18]([O-:20])=[O:19].OS(O)(=O)=O>>[N+:18]([C:12]1[C:11]([CH3:10])=[C:16]([CH:15]=[CH:14][C:13]=1[CH3:17])[CH2:2][NH:3][C:4](=[O:9])[C:5]([F:8])([F:7])[F:6])([O-:20])=[O:19]

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 66722,6-DimethylnitrobenzeneHCID 30849312,2,2-Trifluoro-N-(hydroxymethyl)acetamide

生成物 1

HCID 56840191N-(3-Nitro-2,4-dimethyl-benzyl)-2,2,2-trifluoroacetamide

実験手順

N-(Hydroxymethyl)trifluoroacetamide (6.6 mmol; 0.946 g) is added to a mixture of 2,6-dimethyl-nitrobenzene (0.899 mL; 6.6 mmol) and conc. H2SO4 (15 mL). The mixture is stirred at rt overnight, poured into ice water and stirred for 2 h. The precipitate is collected by filtration and dried. Yield 1.5 g (84%). MS [M−H]−=275, TLC: Rf=0.67 (silica gel, DCM:EtOH 95:5)).

後処理

  1. stirringstirred for 2 h
  2. filtrationThe precipitate is collected by filtration
  3. customdried

出典と根拠

ORDレコード
ord-560eb321dc29451aa32a6678c83af34a
出典データセット
uspto-grants-2013_11
特許番号
US08586604B2

反応ノート

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