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Hydrochloric Acid → 6-Methanesulfonyloxyundecane

HRID 23800
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HRID 23800 반응식
[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]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 31297Methanesulfonyl chlorideHCID 320456-Undecanol

생성물 1

HCID 225905206-Methanesulfonyloxyundecane수율 105%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3b7346425a634f4ba57e2850799830cb
출처 데이터셋
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06852867B2

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