Sodium Hydroxide → Methyl 2-amino-4,6-dimethylbenzoate

HRID 1449558노트

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HRID 1449558 반응식
[OH-].[Na+].[CH3:3][C:4]1[C:9]2[C:10](=[O:15])[O:11][C:12](=O)[NH:13][C:8]=2[CH:7]=[C:6]([CH3:16])[CH:5]=1>CO>[NH2:13][C:8]1[CH:7]=[C:6]([CH3:16])[CH:5]=[C:4]([CH3:3])[C:9]=1[C:10]([O:11][CH3:12])=[O:15]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 189298545,7-Dimethyl-2H-3,1-benzoxazine-2,4(1H)-dione

생성물 1

HCID 18929833Methyl 2-amino-4,6-dimethylbenzoate수율 86%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

To a stirred solution of sodium hydroxide (0.013 g, 0.33 mM) in methanol (1.7 mL) was added 5,7-dimethyl-2H-3,1-benzoxazine-2,4(1H)-dione (0.67 g, 3.5 mM). The mixture was heated to 60° C. and maintained at that temperature for 45 min during which vigorous gas evolution ensued and all solids dissolved completely. The solution was cooled and concentrated using a rotary evaporator. The residue was dissolved in ethyl acetate, and the ethyl acetate solution was washed with water, dried (Na2SO4), filtered and concentrated to provide the title compound (0.54 g, 86%) as a tan solid; MS(CI); 180 (M+H).

후처리

  1. temperaturemaintained at that temperature for 45 min during which vigorous gas evolution
  2. dissolutionall solids dissolved completely
  3. temperatureThe solution was cooled
  4. concentrationconcentrated
  5. customa rotary evaporator
  6. dissolutionThe residue was dissolved in ethyl acetate
  7. washthe ethyl acetate solution was washed with water
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1ad530c606aa4c9887567f0fc65e85cb
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599814

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