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Hydrochloric Acid → 6-Methanesulfonyloxyundecane

HRID 23800
ノート
印刷プレビュー

反応式

HRID 23800 の反応式
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH:6]([OH:12])[CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[CH3:13][S:14](Cl)(=[O:16])=[O:15].Cl>N1C=CC=CC=1>[CH3:13][S:14]([O:12][CH:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])[CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])(=[O:16])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 31297Methanesulfonyl chlorideHCID 320456-Undecanol

生成物 1

HCID 225905206-Methanesulfonyloxyundecane収率 105%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

After dissolving 29.95 g (0.17 mol) of 6-undecanol to 60 mL of pyridine, 29.98 g (0.26 mol) of methanesulfonyl chloride was added dropwise under cooling with ice and the mixture was stirred overnight. Thereafter, 35 mL of 0.5 N aqueous hydrochloric acid was added and the mixture was extracted twice with 200 mL of ethyl acetate. The organic layer was washed with 100 mL of water and a saturated aqueous solution of sodium chloride in that order and thereafter dried over anhydrous magnesium sulfate. After filtering off the magnesium sulfate, the solvent was distilled off to give 44.7 g of 6-methanesulfonyloxy-undecane.

後処理

  1. additionwas added dropwise
  2. temperatureunder cooling with ice
  3. extractionthe mixture was extracted twice with 200 mL of ethyl acetate
  4. washThe organic layer was washed with 100 mL of water
  5. dry with materiala saturated aqueous solution of sodium chloride in that order and thereafter dried over anhydrous magnesium sulfate
  6. filtrationAfter filtering off the magnesium sulfate
  7. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-3b7346425a634f4ba57e2850799830cb
出典データセット
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06852867B2

反応ノート

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