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

HRID 235694

反応式

HRID 235694 の反応式
[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

参加物

4

反応物 2

HCID 240BenzaldehydeHCID 753Glycerol

生成物 1

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

試薬・触媒・溶媒 1

HCID 6101p-Toluenesulfonic acid触媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8d9b652cce9741c6b4cb4ede5852ad0a
出典データセット
uspto-grants-1987_02
特許番号
US04640913

関連ノート

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