Water → Methyl 2-amino-4,6-dimethoxybenzoate

HRID 749186노트

반응식

HRID 749186 반응식
S(OC)(O[CH3:5])(=O)=O.C(=O)([O-])[O-].[K+].[K+].[NH2:14][C:15]1[CH:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([O:26][CH3:27])[C:16]=1[C:17]([OH:19])=[O:18].O>CN(C)C=O>[NH2:14][C:15]1[CH:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([O:26][CH3:27])[C:16]=1[C:17]([O:19][CH3:5])=[O:18]

참가 물질

6

반응물 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 116584562-Amino-4,6-dimethoxybenzoic acid

생성물 1

HCID 11550253Methyl 2-amino-4,6-dimethoxybenzoate수율 77.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Dimethyl sulfate (1.04 ml, 11.0 mmol) was added dropwise to a mixture of potassium carbonate (3.34 g, 24.2 mmol) and 2-amino-4,6-dimethoxybenzoic acid (2.56 g, 11.0 mmol) in dimethylformamide (70 ml) at 0° C. The reaction was stirred for 1 hour, then poured into water. The resulting precipitate was filtered, washed with water and dried in vacuo. The filtrate was extracted with ethyl acetate, and the combined organic extracts were dried (magnesium sulphate) and concentrated in vacuo. The combined solids were dried in vacuo to yield methyl 2-amino-4,6-dimethoxybenzoate (1.8 g, 77% yield) as a yellow crystalline solid:

후처리

  1. filtrationThe resulting precipitate was filtered
  2. washwashed with water
  3. customdried in vacuo
  4. extractionThe filtrate was extracted with ethyl acetate
  5. dry with materialthe combined organic extracts were dried (magnesium sulphate)
  6. concentrationconcentrated in vacuo
  7. customThe combined solids were dried in vacuo

출처 및 근거

ORD 기록
ord-14b32e1043484065b85d5420862f40b1
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07402585B2

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