4-Aminosalicylic Acid → 4-Acetamidosalicylic acid

HRID 1681583

반응식

HRID 1681583 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([OH:11])[C:5](=[CH:9][CH:10]=1)[C:6]([OH:8])=[O:7].[C:12](OC(=O)C)(=[O:14])[CH3:13]>C(O)C>[C:12]([NH:1][C:2]1[CH:3]=[C:4]([OH:11])[C:5](=[CH:9][CH:10]=1)[C:6]([OH:8])=[O:7])(=[O:14])[CH3:13]

참가 물질

4

반응물 2

HCID 46494-Aminosalicylic AcidHCID 7918Acetic Anhydride

생성물 1

HCID 655094-Acetamidosalicylic acid수율 74,088.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred, refluxing suspension of 4-aminosalicylic acid (76.57 g, 0.5 mmol) in 250 mL absolute ethanol was added dropwise, over a 30 minute period, acetic anhydride (83.2 g, 0.815 mmol). After the addition was complete, the mixture was refluxed for another 15 minutes and then cooled. The product collected by filtration, washed with small amount of ethanol and dried on air to give 72.3 g (74.15%) of the title compound as a grey solid mp 242°14 4° C. Previously reported mp: 234°-5° C. (P. Barraclough et al. Eur. J. Chem. 25, p 467, 1990).

후처리

  1. temperatureTo a stirred, refluxing
  2. additionwas added dropwise, over a 30 minute period
  3. additionAfter the addition
  4. temperaturethe mixture was refluxed for another 15 minutes
  5. temperaturecooled
  6. filtrationThe product collected by filtration
  7. washwashed with small amount of ethanol
  8. customdried on air

출처 및 근거

ORD 기록
ord-6720a5e7d7eb4460826c07c0c33658fc
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05173486

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