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

HRID 42669노트

반응식

HRID 42669 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-3428ed0435dc43c99212754307b4a75f
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536203B2

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