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Water → 2-Hydroxyethyl cycloheptyl sulfide

HRID 2186372
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HRID 2186372 반응식
[SH:1][CH2:2][CH2:3][OH:4].[H-].[Na+].Br[CH:8]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.O>CN(C)C=O.C(OCC)C>[CH:8]1([S:1][CH2:2][CH2:3][OH:4])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1
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참가 물질

7

반응물 4

HCID 962WaterHCID 15672-MercaptoethanolHCID 16992BromocycloheptaneHCID 24758Sodium hydride

생성물 1

HCID 224540732-Hydroxyethyl cycloheptyl sulfide수율 92.9%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 6228
Dimethylformamide
용매
3회

실험 절차

2.32 g of 2-mercaptoethanol, dissolved beforehand in 10 cm3 of dimethylformamide, were slowly added, under an inert atmosphere and at a temperature in the region of 20° C., to a stirred suspension of 0.91 g of 60% sodium hydride in 10 cm3 of anhydrous dimethylformamide. After stirring for 20 minutes, 3.5 g of bromocycloheptane, dissolved in 10 cm3 of dimethylformamide, were added. The reaction was brought to completion by stirring at a temperature in the region of 20° C. for 1 hour 30 minutes. The reaction mixture was poured onto 150 cm3 of water to which have been added 100 cm3 of diethyl ether. The ethereal phase was separated by settling and the aqueous phase was extracted once with 50 cm3 of diethyl ether. The organic phases were combined and then washed with 2 times 100 cm3 of water, dried over magnesium sulfate, filtered, and concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 3.2 g of 2-hydroxyethyl cycloheptyl sulfide were obtained in the form of an oil with a yellow color.

후처리

  1. additionwere added
  2. stirringby stirring at a temperature in the region of 20° C. for 1 hour 30 minutes
  3. customThe ethereal phase was separated
  4. extractionthe aqueous phase was extracted once with 50 cm3 of diethyl ether
  5. washwashed with 2 times 100 cm3 of water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C

출처 및 근거

ORD 기록
ord-c15893eda1a044219750fd1658c36fda
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06403610B1

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