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

HRID 648181ノート

反応式

HRID 648181 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].[CH2:10]([CH:12]1[O:14][CH2:13]1)[Cl:11]>N1C=CC=CC=1>[Cl:11][CH2:10][CH:12]([OH:14])[CH2:13][O:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6]

参加物

4

反応物 2

HCID 1013-HydroxybenzaldehydeHCID 7835Epichlorohydrin

生成物 1

HCID 128784723-(3-Chloro-2-hydroxypropoxy)benzaldehyde

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 3-hydroxybenzaldehyde (24.4 g, 0.2 mol), epichlorohydrin (47 ml) and pyridine (0.4 ml) is heated 5 hours on a steam bath. The crude mixture is partitioned between methylenechloride-water and the CH2Cl2 extract washed with dilute aqueous NaHCO3, dried (Na2SO4), filtered and concentrated in vacuo to give the crude title product. Distillation gives a colorless oil bp 160° (0.2 mm); 21.2 g.

後処理

  1. temperatureis heated 5 hours on a steam bath
  2. customThe crude mixture is partitioned between methylenechloride-water
  3. extractionthe CH2Cl2 extract
  4. washwashed with dilute aqueous NaHCO3
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customto give the crude title product
  9. distillationDistillation

出典と根拠

ORDレコード
ord-228ebbddc8eb438a96c0fc17d988e7ed
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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