Formic Acid → 2,4-Dimethyl-3-nitroaniline

HRID 1106729ノート

反応式

HRID 1106729 の反応式
[N+:1]([C:4]1[C:9]([CH3:10])=[CH:8][CH:7]=[C:6]([N+:11]([O-])=O)[C:5]=1[CH3:14])([O-:3])=[O:2].C(O)=O>[Pd].C(N(CC)CC)C.C(OCC)(=O)C>[CH3:14][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[C:9]([CH3:10])[CH:8]=[CH:7][C:6]=1[NH2:11]

参加物

6

反応物 2

HCID 284Formic AcidHCID 690421,3-Dimethyl-2,4-dinitrobenzene

生成物 1

HCID 133699632,4-Dimethyl-3-nitroaniline

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 2,6-dinitro-m-xylene (11.2 g) and 10% palladium on charcoal (620 mg) was stirred in triethylamine (36 mL) under an atmosphere of nitrogen and heated to reflux. Formic acid (9.25 mL) was added dropwise to the above mixture with vigorous stirring. After addition, the mixture was allowed to stir at reflux for an additional 15 min, then cooled to room temperature. The reaction mixture was diluted with ethyl acetate (100 mL) and filtered through celite. The filtrate was washed with brine and dried over magnesium sulfate. Evaporation afforded 9.51 g as a yellow solid.

後処理

  1. temperatureheated to reflux
  2. additionAfter addition
  3. temperatureat reflux for an additional 15 min
  4. filtrationfiltered through celite
  5. washThe filtrate was washed with brine
  6. dry with materialdried over magnesium sulfate
  7. customEvaporation
  8. customafforded 9.51 g as a yellow solid

出典と根拠

ORDレコード
ord-8d2da1e7d1344a998216536d3cd91994
出典データセット
uspto-grants-2000_05
特許番号
US06057349

反応ノート

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