3-(3-Chloro-2-hydroxypropoxy)benzaldehyde → 3-(3-Phthalimido-2-hydroxypropoxy)benzaldehyde

HRID 648182노트

반응식

HRID 648182 반응식
Cl[CH2:2][CH:3]([OH:14])[CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][CH:13]=1)[CH:9]=[O:10].[C:15]1(=[O:25])[NH:19][C:18](=[O:20])[C:17]2=[CH:21][CH:22]=[CH:23][CH:24]=[C:16]12.[K]>CN(C)C=O.CCOCC>[C:15]1(=[O:25])[N:19]([CH2:2][CH:3]([OH:14])[CH2:4][O:5][C:6]2[CH:7]=[C:8]([CH:11]=[CH:12][CH:13]=2)[CH:9]=[O:10])[C:18](=[O:20])[C:17]2=[CH:21][CH:22]=[CH:23][CH:24]=[C:16]12

참가 물질

5

반응물 2

HCID 128784723-(3-Chloro-2-hydroxypropoxy)benzaldehydeHCID 24194345Phthalimide potassium salt

생성물 1

HCID 133240763-(3-Phthalimido-2-hydroxypropoxy)benzaldehyde

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

The distilled product from Example 1 (21.1 g, 0.098 mol) and potassium phthalimide (37 g, 0.20 mol) are dissolved in 100 ml of N,N-dimethylformamide and the mixture is heated 22 hours on a steam bath under N2. The mixture is cooled, diluted with 200 ml of ether and filtered. The filtrate is concentrated to remove ether and diluted to 500 ml with water to give the crystalline title product, 30.8 g, mp 122°-126°.

후처리

  1. temperaturethe mixture is heated 22 hours on a steam bath under N2
  2. temperatureThe mixture is cooled
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated
  5. customto remove ether
  6. additiondiluted to 500 ml with water

출처 및 근거

ORD 기록
ord-996d507d1e094a24afa05537fff04021
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04411899

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