Acetone → phenyl N-methoxy-N-(2-methylphenyl)carbamate

HRID 399783

반응식

HRID 399783 반응식
[C:1](=[O:10])([O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[NH2:2].[C:11]([O-:14])([O-])=O.[K+].[K+].S(OC)(OC)(=O)=O.[CH3:24][C:25]([CH3:27])=O>>[CH3:11][O:14][N:2]([C:24]1[CH:6]=[CH:5][CH:4]=[CH:9][C:25]=1[CH3:27])[C:1](=[O:10])[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

5

반응물 4

HCID 180AcetoneHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 69322Phenyl carbamate

생성물 1

HCID 15767250phenyl N-methoxy-N-(2-methylphenyl)carbamate

실험 절차

A mixture of 2.0 g (8.2 mmol) of the phenyl carbamate from Example 4a, 2 g (15 mmol) of K2CO3 and 1.3 g (10 mmol) of dimethyl sulfate in 20 ml of acetone is stirred for 3 hours at room temperature. The reaction mixture is then filtered and evaporated down, and the residue is purified by column chromatography with mixtures of cyclohexane and ethyl acetate. There is obtained 1.5 g (5.8 mmol =71%) of the title compound as a colorless oil, which slowly crystallizes (mp=60° C.).

후처리

  1. filtrationThe reaction mixture is then filtered
  2. customevaporated down
  3. customthe residue is purified by column chromatography with mixtures of cyclohexane and ethyl acetate

출처 및 근거

ORD 기록
ord-334ac67ec1434702a16820ae73be7012
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05824705

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