Triethylamine → 2-(7-Methoxynaphthalen-1-yl)ethyl methanesulfonate

HRID 2885노트

반응식

HRID 2885 반응식
C(N(CC)CC)C.[S:8](Cl)([CH3:11])(=[O:10])=[O:9].[CH3:13][O:14][C:15]1[CH:24]=[C:23]2[C:18]([CH:19]=[CH:20][CH:21]=[C:22]2[CH2:25][CH2:26][OH:27])=[CH:17][CH:16]=1>ClCCl>[S:8]([O:27][CH2:26][CH2:25][C:22]1[C:23]2[C:18](=[CH:17][CH:16]=[C:15]([O:14][CH3:13])[CH:24]=2)[CH:19]=[CH:20][CH:21]=1)(=[O:10])(=[O:9])[CH3:11]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 135700652-(7-Methoxy-1-naphthyl)ethanol

생성물 1

HCID 190859902-(7-Methoxynaphthalen-1-yl)ethyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-10 °C

실험 절차

In a 250-cm3 flask, 4 g of 2-(7-methoxy-1-naphthyl)ethanol are dissolved in 100 cm3 of dichloromethane, and 3.3 cm3 of triethylamine are added. The mixture is cooled in an ice bath at -10° C. and 2.75 g of mesyl chloride are then added dropwise and with stirring. The mixture is left stirring for 30 minutes. The aqueous phase is extracted with 3 times 50 cm3 of dichloromethane, and the organic phase is washed with 3 times 20 cm3 of 1N hydrochloric acid solution and then with water, dried over potassium carbonate and evaporated. The oily residue is recrystallized.

후처리

  1. waitThe mixture is left
  2. stirringstirring for 30 minutes
  3. extractionThe aqueous phase is extracted with 3 times 50 cm3 of dichloromethane
  4. washthe organic phase is washed with 3 times 20 cm3 of 1N hydrochloric acid solution
  5. dry with materialwith water, dried over potassium carbonate
  6. customevaporated
  7. customThe oily residue is recrystallized

출처 및 근거

ORD 기록
ord-930d75a478a44c1f993455a3cf0bd573
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731352

반응 노트

불러오는 중…