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

HRID 344004노트

반응식

HRID 344004 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-c6656e9d37574e06bc52b4933d3a31c4
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05864046

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