Methylamine → 3,4-Dimethoxy-N-methyl-5-nitrobenzamide

HRID 62013노트

반응식

HRID 62013 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:14]([O-:16])=[O:15])[C:11]=1[O:12][CH3:13])[C:6](Cl)=[O:7].[CH3:17][NH2:18]>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:14]([O-:16])=[O:15])[C:11]=1[O:12][CH3:13])[C:6]([NH:18][CH3:17])=[O:7]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 219286153,4-Dimethoxy-5-nitrobenzoyl chloride

생성물 1

HCID 670370593,4-Dimethoxy-N-methyl-5-nitrobenzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirred solution of 3,4-dimethoxy-5-nitro-benzoyl chloride (0.50 g, 2.04 mmol) in dichloromethane (10 mL) at 0° C., was added dropwise methylamine (1.02 mL, 2.04 mmol, 2 M in THF). The reaction mixture was stirred at room temperature till all starting material disappeared, then diluted with dichloromethane and washed with water. The organic phase was dried over anhydrous magnesium sulphate, filtered and evaporated to dryness to leave a crude residue that was recrystallised from a dichloromethane/isopropanol mixture to afford 3,4-dimethoxy-N-methyl-5-nitro-benzamide, 0.44 g (89%).

후처리

  1. washwashed with water
  2. dry with materialThe organic phase was dried over anhydrous magnesium sulphate
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customto leave a crude residue that
  6. customwas recrystallised from a dichloromethane/isopropanol mixture

출처 및 근거

ORD 기록
ord-0a9522621b304119beaf8ddfb808b019
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09446012B2

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