Acetic Acid → 2-Amino-4,6-dimethylbenzoic acid

HRID 591779

반응식

HRID 591779 반응식
[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[CH:8]=[C:7]2[C:3]=1[C:4](=[O:13])C(=O)[NH:6]2.OO.Cl.C(O)(=[O:19])C>[OH-].[Na+]>[NH2:6][C:7]1[CH:8]=[C:9]([CH3:11])[CH:10]=[C:2]([CH3:1])[C:3]=1[C:4]([OH:13])=[O:19]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 23861614,6-dimethyl-1H-indole-2,3-dione

생성물 1

HCID 133806232-Amino-4,6-dimethylbenzoic acid

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

To a heated (70° C. bath temperature) deep red solution of 4,6-dimethyl-1H-indole-2,3-dione (1.00 g, 5.71 mmol) in 33% aqueous sodium hydroxide (35 mL) was added 35% hydrogen peroxide (3.33 g, 34.3 mmol) over a period of 5 minutes. The reaction mixture was heated for another 15 min, then cooled to room temperature, and ice was added. The pH was adjusted to approximately 8 with concentrated HCl at 0° C. and acidified further to pH approximately 6 with glacial acetic acid. The solid precipitated was filtered, washed well with cold water, and dried under vacuum at 40° C. overnight to obtain 2-amino-4,6-dimethyl-benzoic acid as a pale brown solid. Yield: 0.35 g (37%).

후처리

  1. temperatureThe reaction mixture was heated for another 15 min
  2. additionice was added
  3. customThe solid precipitated
  4. filtrationwas filtered
  5. washwashed well with cold water
  6. customdried under vacuum at 40° C. overnight

출처 및 근거

ORD 기록
ord-a507092f3d674698885eda1e829ff638
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238640B2

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