Hydrochloric Acid → Methyl 3-methylanthranilate

HRID 255856

반응식

HRID 255856 반응식
[NH2:1][C:2]1[C:10]([CH3:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl.[C:13](=O)(O)[O-].[Na+]>CO>[NH2:1][C:2]1[C:10]([CH3:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH3:13])=[O:5]

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 781012-Amino-3-methylbenzoic acidHCID 516892Sodium Bicarbonate

생성물 1

HCID 2763406Methyl 3-methylanthranilate

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
5 °C

실험 절차

A solution of 60.8 g of 2-amino-3-methylbenzoic acid in 900 ml of dry methanol was saturated with anhydrous hydrogen chloride at 0°-10° C., then allowed to stand at room temperature overnight. Then it was refluxed for one hour, cooled to 5° C., resaturated with anhydrous hydrogen chloride, held overnight at room temperature and stripped of solvent. The residue was made neutral with saturated aqueous sodium bicarbonate solution, and extracted with methylene chloride. The extract phase was washed with saturated aqueous sodium bicarbonate solution, dried (MgSO4), filtered and stripped of solvent. The residue was distilled in a kugelrohr apparatus to give methyl 2-amino-3-methylbenzoate (49A), b.p.: 100°-105° C. (1Torr.).

후처리

  1. temperatureThen it was refluxed for one hour
  2. waitheld overnight at room temperature
  3. extractionextracted with methylene chloride
  4. washThe extract phase was washed with saturated aqueous sodium bicarbonate solution
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. distillationThe residue was distilled in a kugelrohr apparatus

출처 및 근거

ORD 기록
ord-5076a2f0ee6f4c48b80060ff58c82f44
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04699651

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