Methanol → Methyl 2-amino-3,5-dichlorobenzoate

HRID 623277노트

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HRID 623277 반응식
[NH2:1][C:2]1[C:10]([Cl:11])=[CH:9][C:8]([Cl:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:18]O>>[CH3:18][O:5][C:4](=[O:6])[C:3]1[CH:7]=[C:8]([Cl:12])[CH:9]=[C:10]([Cl:11])[C:2]=1[NH2:1]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric Acid2회HCID 760363,5-Dichloroanthranilic acid

생성물 1

HCID 613050Methyl 2-amino-3,5-dichlorobenzoate수율 78.6%

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온도
64 °C

실험 절차

To a 500 mL round-bottom flask, 0.2 mol of 2-amino-3,5-dichlorobenzoic acid having a structural formula of IV-4, 300 mL of methanol, and 5 mL of concentrated sulfuric acid were added, heated to 64° C. and reacted for 12 hours (into which 3 mL of concentrated sulfuric acid was added twice), after cooling most of the solvent was removed under reduced pressure, and 300 mL of water was added, the pH was adjusted to 9-10 with a saturated sodium hydroxide solution, extracted with 200 mL of ethyl acetate, washed with water for one time, dried over anhydrous sodium sulfate, filtered and the solvent was remove to obtain a crude product, 34.6 grams of 2-amino-3,5-dichlorobenzoic acid methyl ester having a structure as shown by VIII-1 was obtained by column chromatography, and the yield was 78.6%;

후처리

  1. additionwas added twice),
  2. temperatureafter cooling most of the solvent
  3. customwas removed under reduced pressure, and 300 mL of water
  4. additionwas added
  5. extractionextracted with 200 mL of ethyl acetate
  6. washwashed with water for one time
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. customthe solvent was remove

출처 및 근거

ORD 기록
ord-215dc61984c343fa8353c7f55196dbf9
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09301529B2

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