Triethylamine → 2-(7-Methoxynaphthalen-1-yl)ethyl methanesulfonate

HRID 2885ノート

反応式

HRID 2885 の反応式
C(N(CC)CC)C.[S:8](Cl)([CH3:11])(=[O:10])=[O:9].[CH3:13][O:14][C:15]1[CH:24]=[C:23]2[C:18]([CH:19]=[CH:20][CH:21]=[C:22]2[CH2:25][CH2:26][OH:27])=[CH:17][CH:16]=1>ClCCl>[S:8]([O:27][CH2:26][CH2:25][C:22]1[C:23]2[C:18](=[CH:17][CH:16]=[C:15]([O:14][CH3:13])[CH:24]=2)[CH:19]=[CH:20][CH:21]=1)(=[O:10])(=[O:9])[CH3:11]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 135700652-(7-Methoxy-1-naphthyl)ethanol

生成物 1

HCID 190859902-(7-Methoxynaphthalen-1-yl)ethyl methanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-10 °C

実験手順

In a 250-cm3 flask, 4 g of 2-(7-methoxy-1-naphthyl)ethanol are dissolved in 100 cm3 of dichloromethane, and 3.3 cm3 of triethylamine are added. The mixture is cooled in an ice bath at -10° C. and 2.75 g of mesyl chloride are then added dropwise and with stirring. The mixture is left stirring for 30 minutes. The aqueous phase is extracted with 3 times 50 cm3 of dichloromethane, and the organic phase is washed with 3 times 20 cm3 of 1N hydrochloric acid solution and then with water, dried over potassium carbonate and evaporated. The oily residue is recrystallized.

後処理

  1. waitThe mixture is left
  2. stirringstirring for 30 minutes
  3. extractionThe aqueous phase is extracted with 3 times 50 cm3 of dichloromethane
  4. washthe organic phase is washed with 3 times 20 cm3 of 1N hydrochloric acid solution
  5. dry with materialwith water, dried over potassium carbonate
  6. customevaporated
  7. customThe oily residue is recrystallized

出典と根拠

ORDレコード
ord-930d75a478a44c1f993455a3cf0bd573
出典データセット
uspto-grants-1998_03
特許番号
US05731352

反応ノート

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