p-Toluenesulfonic acid → Chloralose

HRID 1196757ノート

反応式

HRID 1196757 の反応式
[O:1]=[CH:2][C@@H:3]([C@H:5]([C@@H:7]([C@@H:9]([CH2:11][OH:12])[OH:10])[OH:8])[OH:6])[OH:4].O=[CH:14][C:15]([Cl:18])([Cl:17])[Cl:16].CC1C=CC(S(O)(=O)=O)=CC=1>C(Cl)(Cl)Cl>[CH2:11]([OH:12])[C@@H:9]([OH:10])[C@H:7]1[O:8][C@@H:2]2[O:1][C@H:14]([C:15]([Cl:18])([Cl:17])[Cl:16])[O:4][C@@H:3]2[C@H:5]1[OH:6]

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 6407ChloralHCID 107526(2R,3S,4R,5R)-2,3,4,5,6-pentahydroxyhexanal

生成物 1

HCID 7057995Chloralose

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of 4.5 g of glucose, 19 g of chloral, 20 ml of chloroform and 0.05 g of 4-methyl-benzene-sulphonic acid is kept at reflux temperature for 7 hours and the formed water is separated by means of a Dean-Stark apparatus. The solvent is distilled off and the residue is kept at 60° C. for 20 minutes. The sedimented material is filtrated and the pH value of the mother lye adjusted to 6.5 with sodium hydroxide. The separated precipitate is filtered.

後処理

  1. temperatureat reflux temperature for 7 hours
  2. customthe formed water is separated by means of a Dean-Stark apparatus
  3. distillationThe solvent is distilled off
  4. filtrationThe sedimented material is filtrated
  5. filtrationThe separated precipitate is filtered

出典と根拠

ORDレコード
ord-b80a5b8150c544e6ac5f992ebd0d52d2
出典データセット
uspto-grants-1992_05
特許番号
US05116402

反応ノート

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