p-Toluenesulfonic acid → 2-Phenyl-4-(pyrid-3-yl)-5-(2-bromophenyl)-1,3-dioxolane

HRID 1613647ノート

反応式

HRID 1613647 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([OH:17])(O)[CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Br:15])[CH:2]=1.C[O:19][CH:20](OC)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>ClC1C=CC=CC=1.C1(C)C=CC=CC=1>[C:21]1([CH:20]2[O:17][CH:7]([C:3]3[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=3)[CH:8]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[Br:15])[O:19]2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 62375Benzaldehyde dimethyl acetalHCID 197741971-(Pyrid-3-yl)-2-(2-bromophenyl)-ethanediol

生成物 1

HCID 197742082-Phenyl-4-(pyrid-3-yl)-5-(2-bromophenyl)-1,3-dioxolane

試薬・触媒・溶媒 1

HCID 18994452Chlorobenzene toluene溶媒

実験手順

37 g (0.1258 mol) of 1-(pyrid-3-yl)-2-(2-bromophenyl)-ethanediol and 38.5 g (0.2516 mol) of benzaldehyde dimethyl acetal were refluxed together in 440 ml of 10:1 chlorobenzene/toluene with 1 g of p-toluenesulfonic acid. The resulting methanol was distilled off as an azeotrope with toluene. After the end of the reaction, the chlorobenzene was distilled off under reduced pressure and the product wa purified by chromatography over silica gel.

後処理

  1. distillationThe resulting methanol was distilled off as an azeotrope with toluene
  2. customAfter the end of the reaction
  3. distillationthe chlorobenzene was distilled off under reduced pressure
  4. customthe product wa purified by chromatography over silica gel

出典と根拠

ORDレコード
ord-44799372e3b448cca7597c756cfd0536
出典データセット
uspto-grants-1993_03
特許番号
US05194441

反応ノート

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