Pyridine → HCID 178487221, 화합물

HRID 1762571노트

반응식

HRID 1762571 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. additionare then added
  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-9f95fbf3c09649bba2cdbaab75ff1467
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04833169

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