Triethylamine → Methanesulfonic acid 3-benzenesulfonyl-3-methylbutyl ester

HRID 2212070ノート

反応式

HRID 2212070 の反応式
[C:1]1([S:7]([C:10]([CH3:15])([CH3:14])[CH2:11][CH2:12][OH:13])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[CH3:23][S:24](Cl)(=[O:26])=[O:25]>>[C:1]1([S:7]([C:10]([CH3:15])([CH3:14])[CH2:11][CH2:12][O:13][S:24]([CH3:23])(=[O:26])=[O:25])(=[O:8])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 149069793-Benzenesulfonyl-3-methyl-butan-1-ol

生成物 1

HCID 86595010Methanesulfonic acid 3-benzenesulfonyl-3-methylbutyl ester収率 103.1%

実験手順

A solution of 3-benzenesulfonyl-3-methyl-butan-1-ol (2.17 g, 9.5 mmol), triethylamine (2.0 ml, 14.25 mmol), methanesulphonyl chloride (0.9 ml, 11.78 mmol) and 4-N,N-dimethylaminopyridine (12 mg, 0.01 mmol) was stirred at 0° C. for 45 min. After quenching with satd. NaHCO3, the mixture was extracted into dichloromethane. The combined organic extracts were dried (Na2SO4) and concentrated to give the title product (3.0 g).

後処理

  1. customAfter quenching with satd
  2. extractionNaHCO3, the mixture was extracted into dichloromethane
  3. dry with materialThe combined organic extracts were dried (Na2SO4)
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-4f69f1bcb9d44b4b9564223aaaf7654c
出典データセット
uspto-grants-2006_09
特許番号
US07101892B2

反応ノート

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