Water → 6-Camphenol

HRID 1980459ノート

反応式

HRID 1980459 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 24386Thionyl ChlorideHCID 13493472HCID 13493472、化合物

生成物 1

HCID 1805376-Camphenol収率 6.6%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-abc7af828dec49a28d8e545b199944fa
出典データセット
uspto-grants-1985_04
特許番号
US04510025

反応ノート

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