p-Toluenesulfonic acid → Chloralose

HRID 1196757노트

반응식

HRID 1196757 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 7057995Chloralose

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b80a5b8150c544e6ac5f992ebd0d52d2
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05116402

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