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

HRID 551775

반응식

HRID 551775 반응식
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]=[CH:8][CH:9]=[C:10]2[CH2:13][CH2:14][OH:15])=[CH:5][CH:4]=1.C(N(CC)CC)C.[S:23](Cl)([CH3:26])(=[O:25])=[O:24].O>ClCCl>[CH3:26][S:23]([O:15][CH2:14][CH2:13][C:10]1[C:11]2[C:6](=[CH:5][CH:4]=[C:3]([O:2][CH3:1])[CH:12]=2)[CH:7]=[CH:8][CH:9]=1)(=[O:25])=[O:24]

참가 물질

6

반응물 4

HCID 962WaterHCID 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
0 °C

실험 절차

2-(7-Methoxy-1-naphthyl)ethanol (25 mmol) and triethylamine (30 mmol) are dissolved in 50 ml of dichloromethane and the reaction mixture is cooled to 0° C. using an ice bath. Mesyl chloride (30 mmol) is added dropwise and the reaction mixture is stirred at ambient temperature for 2 hours and then poured into 100 ml of water. The organic phase is washed with 1M hydrochloric acid solution and then with water, dried over magnesium sulphate and evaporated. The oil obtained is precipitated from a mixture of diethyl ether/petroleum ether (1/1). The title product is filtered off under suction and then recrystallised from to diisopropyl ether.

후처리

  1. washThe organic phase is washed with 1M hydrochloric acid solution
  2. dry with materialwith water, dried over magnesium sulphate
  3. customevaporated
  4. customThe oil obtained
  5. customis precipitated from a mixture of diethyl ether/petroleum ether (1/1)
  6. filtrationThe title product is filtered off under suction
  7. customrecrystallised from to diisopropyl ether

출처 및 근거

ORD 기록
ord-3ed8828f72094897973923c2cbadfc7a
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947852B2

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