Benzaldehyde → 1,3-Dioxan-5-ol, 2-phenyl-

HRID 235694노트

반응식

HRID 235694 반응식
[CH:1](=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH:9][CH2:10][CH:11]([CH2:13]O)[OH:12]>C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:2]1([CH:1]2[O:9][CH2:10][CH:11]([OH:12])[CH2:13][O:8]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 240BenzaldehydeHCID 753Glycerol

생성물 1

HCID 743621,3-Dioxan-5-ol, 2-phenyl-수율 21.1%

시약·촉매·용매 1

HCID 6101p-Toluenesulfonic acid촉매

반응 조건

온도
0 °C

실험 절차

A mixture of about 184 g of glycerol, about 212.03 g of benzaldehyde and about 3.6 g of p-toluenesulfonic acid was refluxed for about 5 hours, using a Dean-Stark trap. The mixture was then cooled at about 0° C. for about 17 hours and the solid collected and dissolved in about 1200 ml of warm toluene containing about one gram of sodium methoxide. This solution was washed with about 600 ml of dilute (about 1%) dibasic sodium phosphate and dried. Dilution with petroleum ether gave a solid which was recrystallized from toluene-petroleum ether, giving about 76 g of the desired title compound as a white solid.

후처리

  1. temperaturewas refluxed for about 5 hours
  2. customthe solid collected
  3. dissolutiondissolved in about 1200 ml of warm toluene containing about one gram of sodium methoxide
  4. washThis solution was washed with about 600 ml
  5. additionof dilute (about 1%) dibasic sodium phosphate
  6. customdried
  7. customDilution with petroleum ether gave a solid which
  8. customwas recrystallized from toluene-petroleum ether

출처 및 근거

ORD 기록
ord-8d9b652cce9741c6b4cb4ede5852ad0a
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04640913

반응 노트

불러오는 중…