Phosphorus pentachloride → 3,4-Dimethoxy-N-methyl-5-nitro-benzimidoyl chloride

HRID 62014ノート

反応式

HRID 62014 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([N+:15]([O-:17])=[O:16])[C:12]=1[O:13][CH3:14])[C:6]([NH:8][CH3:9])=O.P(Cl)(Cl)(Cl)(Cl)[Cl:19]>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([N+:15]([O-:17])=[O:16])[C:12]=1[O:13][CH3:14])[C:6]([Cl:19])=[N:8][CH3:9]

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 670370593,4-Dimethoxy-N-methyl-5-nitrobenzamide

生成物 1

HCID 866431073,4-Dimethoxy-N-methyl-5-nitro-benzimidoyl chloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a stirred suspension of 3,4-dimethoxy-N-methyl-5-nitro-benzamide (0.40 g, 1.66 mmol) in toluene (10 mL) was added phosphorous pentachloride (0.28 g, 1.83 mmol) portionwise. Upon completion of addition, the reaction mixture was warmed to reflux till complete disappearance of starting material. Evaporation to dryness resulted in a crude solid that was washed with diethyl ether, affording 3,4-dimethoxy-N-methyl-5-nitro-benzimidoyl chloride, 0.37 g (85%).

後処理

  1. additionUpon completion of addition
  2. temperaturethe reaction mixture was warmed
  3. temperatureto reflux till complete disappearance of starting material
  4. customEvaporation to dryness
  5. customresulted in a crude solid
  6. washthat was washed with diethyl ether

出典と根拠

ORDレコード
ord-ae1719c0be7943d484586798cdb9d41f
出典データセット
uspto-grants-2016_09
特許番号
US09446012B2

反応ノート

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