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

HRID 1613647노트

반응식

HRID 1613647 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 18994452Chlorobenzene toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-44799372e3b448cca7597c756cfd0536
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194441

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