Triethylamine → Methanesulphonic acid 2-(6-methoxyindan-1-yl)ethyl ester

HRID 2165163ノート

反応式

HRID 2165163 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][CH:9]2[CH2:12][CH2:13][OH:14])=[CH:5][CH:4]=1.[CH3:15][S:16](Cl)(=[O:18])=[O:17].C(N(CC)CC)C>ClCCl>[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][CH:9]2[CH2:12][CH2:13][O:14][S:16]([CH3:15])(=[O:18])=[O:17])=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 109978572-(6-Methoxyindan-1-yl)ethanol

生成物 1

HCID 53897303Methanesulphonic acid 2-(6-methoxyindan-1-yl)ethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5.0 g (26.0 mmol) of crude 2-(6-methoxyindan-1-yl)ethanol are dissolved in 50 ml of dichloromethane and, while cooling with ice, 3.6 g (31 mmol) of methanesulphonic acid chloride and 3.1 g (31 mmol) of triethylamine are added dropwise. The mixture is stirred at room temperature for 3 hours, the triethyl-ammonium chloride which has precipitated is filtered off and the filtrate is extracted by shaking with ice-water. The organic phases are washed with saturated sodium chloride solution, dried over magnesium sulphate and concentrated by evaporation at 40° under reduced pressure. Methanesulphonic acid 2-(6-methoxyindan-1-yl)ethyl ester is obtained which can be used without further purification.

後処理

  1. additionare added dropwise
  2. customthe triethyl-ammonium chloride which has precipitated
  3. filtrationis filtered off
  4. extractionthe filtrate is extracted
  5. stirringby shaking with ice-water
  6. washThe organic phases are washed with saturated sodium chloride solution
  7. dry with materialdried over magnesium sulphate
  8. concentrationconcentrated by evaporation at 40° under reduced pressure

出典と根拠

ORDレコード
ord-871f2c4bb909424ebaf0570de3cdfbef
出典データセット
uspto-grants-1990_07
特許番号
US04939160

反応ノート

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