Potassium Hydroxide → 2-Chloro-3,5-Dimethoxyaniline

HRID 58176

반응식

HRID 58176 반응식
[OH-].[K+].[Cl:3][C:4]1[C:9]([O:10][CH3:11])=[CH:8][C:7]([O:12][CH3:13])=[CH:6][C:5]=1[NH:14]C(=O)C>CCO.O>[Cl:3][C:4]1[C:9]([O:10][CH3:11])=[CH:8][C:7]([O:12][CH3:13])=[CH:6][C:5]=1[NH2:14]

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 56594868N-(2-chloro-3,5-dimethoxyphenyl)acetamide

생성물 1

HCID 227430742-Chloro-3,5-Dimethoxyaniline수율 82%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Potassium hydroxide (2.19 g, 39.18 mmol) was added to a solution of N-(2-chloro-3,5-dimethoxyphenyl)acetamide (1.8 g, 7.837 mmol) in EtOH (100 mL) and water (10 mL) and the reaction mixture heated to reflux for 12 h. Excess EtOH was removed under reduced pressure to obtain a residue. The residue was then partitioned between water and diethyl ether. The organic layer was separated, dried over sodium sulfate, filtered and concentrated under vacuum to afford the title compound (1.2 g, 82% of yield) as a white solid. 1HNMR (CDCl3, 300 MHz): δ 5.97 (s, 2H), 4.08 (brs, 2H), 3.84 (s, 3H), 3.75 (s, 3H); MS (ESI): 188.1 [M+H]+.

후처리

  1. temperaturethe reaction mixture heated
  2. temperatureto reflux for 12 h
  3. customExcess EtOH was removed under reduced pressure
  4. customto obtain a residue
  5. customThe residue was then partitioned between water and diethyl ether
  6. customThe organic layer was separated
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-e54c098ae5e44c79abbbc706661fc090
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434697B2

연결된 노트

불러오는 중…