Hydrochloric Acid → 2-(2-Methanesulfonyloxyethyl)-5,6,7-trimethoxynaphthalene

HRID 987420노트

반응식

HRID 987420 반응식
[OH:1][CH2:2][CH2:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][C:8]([O:18][CH3:19])=[C:9]([O:16][CH3:17])[C:10]=2[O:14][CH3:15])[CH:5]=1.[CH3:20][S:21](Cl)(=[O:23])=[O:22].Cl>N1C=CC=CC=1>[CH3:20][S:21]([O:1][CH2:2][CH2:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][C:8]([O:18][CH3:19])=[C:9]([O:16][CH3:17])[C:10]=2[O:14][CH3:15])[CH:5]=1)(=[O:23])=[O:22]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 31297Methanesulfonyl chlorideHCID 218915912-(2-Hydroxyethyl)-5,6,7-trimethoxynaphthalene

생성물 1

HCID 218915682-(2-Methanesulfonyloxyethyl)-5,6,7-trimethoxynaphthalene

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2-(2-Hydroxyethyl)-5,6,7-trimethoxynaphthalene (1.26 g) was dissolved in pyridine (5 mL), methanesulfonyl chloride (715 mg) was added at 0° C. to the solution, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was acidified with hydrochloric acid and extracted with ethyl acetate. The resultant extract was washed with water and saturated brine. The solvent was distilled off under reduced pressure, and the residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:5) to obtain the title compound.

후처리

  1. extractionextracted with ethyl acetate
  2. extractionThe resultant extract
  3. washwas washed with water and saturated brine
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:5)

출처 및 근거

ORD 기록
ord-fdf21c993a7944ab8c2f4e1f9167b102
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06632810B2

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