Pyridine → HCID 178487221, 화합물

HRID 2165149노트

반응식

HRID 2165149 반응식
N1C=CC=CC=1.[CH3:7][S:8](Cl)(=[O:10])=[O:9].[CH3:12][O:13][C:14]1[CH:15]=[CH:16][C:17]2[CH:20]=[C:19]([CH2:21][OH:22])[C:18]=2[CH:23]=1>ClCCl>[CH3:12][O:13][C:14]1[CH:15]=[CH:16][C:17]2[CH:20]=[C:19]([CH2:21][O:22][S:8]([CH3:7])(=[O:10])=[O:9])[C:18]=2[CH:23]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 23044250HCID 23044250, 화합물

생성물 1

HCID 178487221HCID 178487221, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

6.1 ml (76 mmol) of pyridine and 3.6 ml (46 mmol) of methanesulphonic acid chloride are added at 0° C., while stirring, with the exclusion of moisture, to 5.0 g (30.5 mmol) of (5-methoxybenzocyclobuten-1-yl)methanol in 50 ml of dichloromethane. The mixture is then stirred at room temperature for a further 18 hours to complete the reaction. 50 ml of ice-water are then added and the whole is stirred for 30 minutes. The organic phase is separated off, washed once in each case with 2N sodium hydroxide solution, 2N hydrochloric acid and water, dried over sodium sulphate and concentrated under reduced pressure. Methanesulphonic acid (5-methoxybenzocyclobuten-1-ylmethyl) ester is obtained in the form of a viscous oil, Rf=0.4, toluene/ethyl acetate (9:1).

후처리

  1. customthe reaction
  2. stirringthe whole is stirred for 30 minutes
  3. customThe organic phase is separated off
  4. washwashed once in each case with 2N sodium hydroxide solution, 2N hydrochloric acid and water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-69970ee26a5d4be0bf1a2fce2bdb40d8
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04939160

반응 노트

불러오는 중…