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Hydrochloric Acid → HCID 13946785, 화합물

HRID 1863524
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HRID 1863524 반응식
COC([CH:5]1[CH:9]([CH:10]([S:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)/[CH:11]=[CH:12]/[CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH2:8][O:7][C:6]1=[O:25])=O.[Cl-].[Li+].Cl>CN(C)P(=O)(N(C)C)N(C)C>[C:19]1([S:18][CH:10]([CH:9]2[CH2:8][O:7][C:6](=[O:25])[CH2:5]2)/[CH:11]=[CH:12]/[CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 433294Lithium ChlorideHCID 20392009HCID 20392009, 화합물

생성물 1

HCID 13946785HCID 13946785, 화합물

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매

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온도
100 °C

실험 절차

60 mg (0.17 mmol) of 3-methoxycarbonyl-4-(1-phenylthio-trans-2-octenyl)-oxolane-2-one was dissolved in 2 ml of hexamethyl phosphoric triamide in an argon atmosphere, and 36 mg (0.85 mmol) of lithium chloride was added to the solution followed by heating at a temperature of 100° C. for 5 hours with stirring. The reaction mixture was then allowed to cool to room temperature and decomposed with dilute hydrochloric acid. The mixture was extracted with ethyl acetate, and the extract was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The mixture was filtered and the filtrated was concentrated under reduced pressure. The resulting residue was then purified by silica gel column chromatography to obtain 4-(1-phenylthio-trans-2-octenyl)-oxolane-2-one.

후처리

  1. additionwas added to the solution
  2. temperatureto cool to room temperature
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe extract was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationThe mixture was filtered
  7. concentrationthe filtrated was concentrated under reduced pressure
  8. customThe resulting residue was then purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-72a5f5b514a5431ea64686ad37628917
출처 데이터셋
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04169199

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