Acetic Acid → 4-(3,4-Dimethoxyphenyl)-4-oxobutanoic acid

HRID 482007

반응식

HRID 482007 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11](=[O:16])[CH2:12]CC#N)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[C:17]([OH:20])(=[O:19])[CH3:18]>Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11](=[O:16])[CH2:12][CH2:18][C:17]([OH:20])=[O:19])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 124916314-(3,4-Dimethoxyphenyl)-4-oxobutanenitrile

생성물 1

HCID 2193904-(3,4-Dimethoxyphenyl)-4-oxobutanoic acid

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A stirred solution of 4-(3',4'-dimethoxyphenyl)-4-oxobutyronitrile (111) (2.26 g, 0.01 mol) in acetic acid (15 ml) and hydrochloric acid (12N, 40 ml) was heated at reflux for 1.5 hours and cooled to room temperature. The solvent was removed under reduced pressure to give a brown solid. Recrystallization from water gave 112 as light tan crystals (1.57 g, 66%). 1H NMR (CDCl3) 2.80 (t, J=7.5 Hz, 2H), 3.30 (t, J=7.5 Hz, 2H), 3.94 (s, 3H), 3.96 (s, 3H), 6.89 (d, 1H, J=9 Hz), 7.55 (d, 1H, J=1 Hz) and 7.64 (dd, 1H, 1 and 9 Hz).

후처리

  1. temperatureat reflux for 1.5 hours
  2. customThe solvent was removed under reduced pressure
  3. customto give a brown solid
  4. customRecrystallization from water

출처 및 근거

ORD 기록
ord-a3430dbd91cd4846a6af4030c3ab5be6
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05792776

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