Water → 9-(2-Hydroxyethyl)-7, 11-dioxaspiro[5,5]undecane

HRID 2354ノート

反応式

HRID 2354 の反応式
[OH:1][CH2:2][CH:3]1[CH2:14][CH2:13][O:12][C:6]2([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[O:5][CH2:4]1.C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1C=CC=CC=1>[OH:12][CH2:13][CH2:14][CH:3]1[CH2:2][O:1][C:6]2([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[O:5][CH2:4]1

参加物

5

反応物 3

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 110308447,12-Dioxaspiro[5.6]dodecane-9-methanol

生成物 1

HCID 108673469-(2-Hydroxyethyl)-7, 11-dioxaspiro[5,5]undecane

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 9-hydroxymethyl-7, 12-dioxaspiro[5,6]dodecane of the formula V (4 g) of the drawings in benzene (15 ml) was stirred at 10° C. for 5 hr with anhydrous p-toluenesulphonic acid (0.2 g). The reaction mixture was made alkaline by adding TEA and water. The benzene layer was separated and the aqueous layer extracted with benzene. The combined benzene solution was dried over K2CO3 and evaporate to a residue (4 g). It was chromatograped on silicagel using chloroform-methanol mixture as eluent to give 9-(2-hydroxyethyl)-7, 11-dioxaspiro[5,5]undecane of formula VI (2.8 g) (70%) of the drawings as colorless viscous liquid.

後処理

  1. customThe benzene layer was separated
  2. extractionthe aqueous layer extracted with benzene
  3. dry with materialThe combined benzene solution was dried over K2CO3
  4. customevaporate to a residue (4 g)

出典と根拠

ORDレコード
ord-41c36e816c8a49348cb7de1b22c2c650
出典データセット
uspto-grants-1998_03
特許番号
US05728848

反応ノート

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