Ammonia → 3-Methoxy-2-methylbenzamide

HRID 1760723노트

반응식

HRID 1760723 반응식
[CH3:1][O:2][C:3]1[C:4]([CH3:12])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6](O)=[O:7].C1C=CC2N(O)N=[N:19]C=2C=1.N>C(Cl)Cl.CN(C=O)C>[CH3:1][O:2][C:3]1[C:4]([CH3:12])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([NH2:19])=[O:7]

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 757711-HydroxybenzotriazoleHCID 70214833-Methoxy-2-MethylBenzoic Acid

생성물 1

HCID 160946953-Methoxy-2-methylbenzamide수율 58.5%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

3-Methoxy-2-methylbenzoic acid (5.0 g, 30 mmol) in CH2Cl2 (90 ml) and DMF (90 ml) was treated with HOBt (4.06 g, 30 mmol) and WSCDI (5.75 g, 30 mmol) and the resulting mixture stirred at RT for 20 min. After cooling to 0° C. ammonia (2H in EtOH, 30 ml, 60 mmol) was added and the mixture stirred for a further 2 h. The mixture was filtered, the solvent was removed from the filtrate. The crude material was taken up in CH2Cl2 and washed with water and brine and dried (Na2SO4), which gave a white solid (2.9 g) on isolation.

후처리

  1. additionwas added
  2. stirringthe mixture stirred for a further 2 h
  3. filtrationThe mixture was filtered
  4. customthe solvent was removed from the filtrate
  5. washwashed with water and brine
  6. dry with materialdried (Na2SO4), which

출처 및 근거

ORD 기록
ord-dbac52c2bb1b4c1ea2e25c87c21c6b30
출처 데이터셋
uspto-grants-2005_01
특허 번호
US06844362B2

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