Dimethylformamide → 3-Methyl-2-nitrobenzamide

HRID 128995

반응식

HRID 128995 반응식
C(Cl)(=O)C(Cl)=O.[N+:7]([C:10]1[C:18]([CH3:19])=[CH:17][CH:16]=[CH:15][C:11]=1[C:12](O)=[O:13])([O-:9])=[O:8].C[N:21](C)C=O>C(Cl)Cl>[CH3:19][C:18]1[C:10]([N+:7]([O-:9])=[O:8])=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12]([NH2:21])=[O:13]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 215753-Methyl-2-nitrobenzoic acidHCID 65578Oxalyl chloride

생성물 1

HCID 32713713-Methyl-2-nitrobenzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Oxalyl chloride (18.1 ml, 36.1 mmol, 1.25 eq., 2M in CH2Cl2) was added to a solution of 2-nitro-3-methyl-benzoic acid (5.237 g, 28.9 mmol, 1.0 eq.) in CH2Cl2 (57.8 ml, 0.5M) and dimethylformamide (0.14 ml, 0.25% of CH2Cl2) at 0° C. and stirred for 15 minutes. The reaction was then warmed to room temperature and stirred for 3 hours. Ammonia was bubbled through the reaction for 30 minutes. Water was then added. The product was filtered off ,and pumped on to provide the title A compound (3.81 g).

후처리

  1. stirringstirred for 3 hours
  2. customAmmonia was bubbled through the reaction for 30 minutes
  3. additionWater was then added
  4. filtrationThe product was filtered off

출처 및 근거

ORD 기록
ord-bf8d878ef1da413ea52d59b3b398071f
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05466704

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