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

HRID 720312ノート

反応式

HRID 720312 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-35c27692af2a4e24ba93457262bbdadc
出典データセット
uspto-grants-2006_11
特許番号
US07135473B2

反応ノート

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