Water → 6-Camphenol

HRID 1980459노트

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HRID 1980459 반응식
[CH3:1][C:2]1([CH3:12])[C:7]([CH3:9])(O)[CH:6]2[CH2:10][CH:3]1[CH2:4][CH:5]2[OH:11].S(Cl)(Cl)=O.O>N1C=CC=CC=1>[CH3:1][C:2]1([CH3:12])[C:7](=[CH2:9])[C@H:6]2[C@H:5]([OH:11])[CH2:4][C@@H:3]1[CH2:10]2

참가 물질

5

반응물 3

HCID 962WaterHCID 24386Thionyl ChlorideHCID 13493472HCID 13493472, 화합물

생성물 1

HCID 1805376-Camphenol수율 6.6%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

In 5.0 ml of pyridine was dissolved 1.7 g of 2,2,3-trimethylbicyclo[2.2.1]heptan-3,5-diol and, then, 1.2 g of thionyl chloride was added dropwise to the solution at a temperature of -5° C. to 0° C. The mixture was stirred for 2 hours, after which it was poured into water and extracted with n-hexane. The extract was washed with dilute hydrochloric acid and an aqueous solution of sodium hydrogen carbonate in that order, dried over anhydrous magnesium sulfate, and distilled to remove the hexane. The residue was subjected to silica gel column chromatography to give 0.10 g of nojigiku alcohol. The physical properties of this product were in agreement with those of the nojigiku alcohol obtained in Example 1.

후처리

  1. extractionextracted with n-hexane
  2. washThe extract was washed with dilute hydrochloric acid
  3. dry with materialan aqueous solution of sodium hydrogen carbonate in that order, dried over anhydrous magnesium sulfate
  4. distillationdistilled
  5. customto remove the hexane

출처 및 근거

ORD 기록
ord-abc7af828dec49a28d8e545b199944fa
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04510025

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