Dimethyl Sulfate → Benzoic acid, 2-(methylamino)-3-nitro-, methyl ester

HRID 23908

반응식

HRID 23908 반응식
[CH3:1][NH:2][C:3]1[CH:11]=[CH:10][C:6](C(O)=O)=[CH:5][C:4]=1[N+:12]([O-:14])=[O:13].[C:15]([O-:18])([O-])=[O:16].[K+].[K+].S(OC)(O[CH3:25])(=O)=O>CN(C)C=O.O>[CH3:25][O:18][C:15](=[O:16])[C:11]1[CH:10]=[CH:6][CH:5]=[C:4]([N+:12]([O-:14])=[O:13])[C:3]=1[NH:2][CH3:1]

참가 물질

6

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 2834754-(Methylamino)-3-nitrobenzoic acid

생성물 1

HCID 59635415Benzoic acid, 2-(methylamino)-3-nitro-, methyl ester

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

9.8 g (50 mmol) of 4-methylamino-3-nitro-benzoic acid are treated in 50 ml of dimethyl formamide (DMF) with K2CO3 (14 g). 5 ml of dimethyl sulphate are added dropwise to this mixture over 10 minutes with stirring. It is stirred for 15 minutes and heated for 0.5 hours at 60° C. After cooling, it is diluted with water, the precipitated solids are filtered off, washed with water and dried. Yield: 9.8 g (93%); M.Pt.: 138-140° C.

후처리

  1. stirringIt is stirred for 15 minutes
  2. temperatureAfter cooling
  3. filtrationthe precipitated solids are filtered off
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-2a1b0aad832c47bf93263209157fb435
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06855713B2

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