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Water → 5,6-Dihydro-5,5-dimethyl-4H-1,3,2-dioxathiin 2-oxide

HRID 467296
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HRID 467296 반응식
[CH3:1][C:2]([CH3:7])([CH2:5][OH:6])[CH2:3][OH:4].[S:8](Cl)(Cl)=[O:9].O>C(Cl)Cl>[CH3:1][C:2]1([CH3:7])[CH2:5][O:6][S:8](=[O:9])[O:4][CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24386Thionyl ChlorideHCID 31344Neopentyl glycol

생성물 1

HCID 108772945,6-Dihydro-5,5-dimethyl-4H-1,3,2-dioxathiin 2-oxide수율 92%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

25.36 g (0.24 mol) of 2,2-dimethylpropane-1,3-diol was suspended at room temperature in 150 ml of methylene chloride in a 500 ml three-necked flask. 37.36 g (0.31 mol) of thionyl chloride was instilled over 30 minutes. After the end of the addition, the reaction solution was held at reflux for 1.5 hours and then cooled to room temperature. 100 ml of water was added to the reaction. The aqueous phase was discarded; the organic phase was extracted three times with saturated NaHCO3 solution (100 ml), then dried with Na2SO4 and concentrated by evaporation on a rotary evaporator. The residue was distilled at 24 mbars and 78° C. The product was a pure colorless liquid according to GC and weighed 23.4 g, which corresponded to a yield of 92 percent.

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후처리

  1. additionAfter the end of the addition
  2. temperatureat reflux for 1.5 hours
  3. extractionthe organic phase was extracted three times with saturated NaHCO3 solution (100 ml)
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated by evaporation on a rotary evaporator
  6. distillationThe residue was distilled at 24 mbars and 78° C

출처 및 근거

ORD 기록
ord-92b509c9928a459bbfa1c5331f1933d0
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05159100

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