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

HRID 1449558ノート

反応式

HRID 1449558 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 18929833Methyl 2-amino-4,6-dimethylbenzoate収率 86%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1ad530c606aa4c9887567f0fc65e85cb
出典データセット
uspto-grants-1997_02
特許番号
US05599814

反応ノート

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