Hydrochloric Acid → 1-(5-Amino-2-methoxyphenyl)ethanone

HRID 1870231노트

반응식

HRID 1870231 반응식
Cl.[C:2]([C:5]1[CH:6]=[C:7]([NH:13]C(=O)C)[CH:8]=[CH:9][C:10]=1[O:11][CH3:12])(=[O:4])[CH3:3]>C(O)C>[NH2:13][C:7]1[CH:8]=[CH:9][C:10]([O:11][CH3:12])=[C:5]([C:2](=[O:4])[CH3:3])[CH:6]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 28174183-Acetyl-4-methoxyacetanilide

생성물 1

HCID 155794431-(5-Amino-2-methoxyphenyl)ethanone수율 99%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Hydrochloric acid (6M, 50 ml) was added to a mixture of N-(3-acetyl-4-methoxyphenyl)acetamide (10.34 g, 50 mmol) and ethanol (150 ml) and the mixture was stirred under reflux for 8 hours. The mixture was cooled and the solvent was evaporated under reduced pressure. Water (100 ml) was added and the pH was adjusted to 10.0 with saturated aqueous potassium carbonate. The mixture was extracted with dichloromethane (3×100 ml) and the combined organic fractions were dried (MgSO4) and evaporated under reduced pressure to give 1-(5-amino-2-methoxyphenyl)ethanone as a dark oil (8.16 g, 99%), 1H NMR (CDCl3) δ 7.09 (1H, d, J=2.8 Hz), 6.82 (2H, m), 3.84 (3H, s), and 3.34 (2H, br. s), 2.59 (3H, s). m/e (CI+) 166 (MH+).

후처리

  1. temperatureunder reflux for 8 hours
  2. temperatureThe mixture was cooled
  3. customthe solvent was evaporated under reduced pressure
  4. additionWater (100 ml) was added
  5. extractionThe mixture was extracted with dichloromethane (3×100 ml)
  6. dry with materialthe combined organic fractions were dried (MgSO4)
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-39087a7182c54c0ba1cf02090bca77d2
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06096766

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