Imidazole → (But-3-yn-1-yloxy)(tert-butyl)dimethylsilane

HRID 462382

반응식

HRID 462382 반응식
[CH2:1]([OH:5])[CH2:2][C:3]#[CH:4].N1C=CN=C1.[Si:11](Cl)([C:14]([CH3:17])([CH3:16])[CH3:15])([CH3:13])[CH3:12]>CN(C)C=O>[Si:11]([O:5][CH2:1][CH2:2][C:3]#[CH:4])([C:14]([CH3:17])([CH3:16])[CH3:15])([CH3:13])[CH3:12]

참가 물질

5

반응물 3

HCID 795ImidazoleHCID 135663-Butyn-1-OLHCID 28928tert-Butyldimethylsilyl chloride

생성물 1

HCID 4304567(But-3-yn-1-yloxy)(tert-butyl)dimethylsilane수율 86.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 21 g of 3-butyn-1-ol and 27 g of imidazole in 100 ml of dimethyl formamide was treated with 45 g of t-butyldimethylsilyl chloride in several portions over a one hour period. After stirring under nitrogen for 18 hours the reaction mixture was diluted with 500 ml of ice water. The resulting aqueous solution was extracted with 300 ml of ether and the ethereal solution washed with water and then brine. The ethereal solution was dried over potassium carbonate. Evaporation of the ether and distillation of the residue gave 47.6 g of 3-butyn-1-ol t-butyldimethylsilyl ether, bp 80°-83° C./25 mm.

후처리

  1. extractionThe resulting aqueous solution was extracted with 300 ml of ether
  2. washthe ethereal solution washed with water
  3. dry with materialThe ethereal solution was dried over potassium carbonate
  4. customEvaporation of the ether and distillation of the residue

출처 및 근거

ORD 기록
ord-5e65622494834595801ef6ba7857a3f8
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04515727

연결된 노트

불러오는 중…