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

HRID 648182ノート

反応式

HRID 648182 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-996d507d1e094a24afa05537fff04021
出典データセット
uspto-grants-1983_10
特許番号
US04411899

反応ノート

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