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Hydrazine → Oxane-4-carbohydrazide

HRID 710943
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HRID 710943 반응식
[O:1]1[CH2:6][CH2:5][CH:4]([C:7]([O:9]C)=O)[CH2:3][CH2:2]1.[NH2:11][NH2:12]>CO>[O:1]1[CH2:6][CH2:5][CH:4]([C:7]([NH:11][NH2:12])=[O:9])[CH2:3][CH2:2]1
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참가 물질

4

반응물 2

HCID 9321HydrazineHCID 27735202H-Pyran-4-carboxylic acid, tetrahydro-, methyl ester

생성물 1

HCID 28064717Oxane-4-carbohydrazide수율 66.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of methyl tetrahydro-2H-pyran-4-carboxylate (1.44 g, 10.0 mmol) in methanol (50 mL) was stirred at 50° C. To the reaction mixture, hydrazine.monohydrate (0.675 g) was added, followed by stirring at the same temperature for 2 hours, after completion of the reaction, the reaction mixture was concentrated and diluted with methylene chloride, the solution was then washed with saturated sodium bicarbonate aqueous solution and saturated brine, and the organic layer was dried over magnesium sulfate and the solvent was distilled off under reduced pressure to afford 952 mg of the title compound (yield 66.1%).

후처리

  1. customafter completion of the reaction
  2. concentrationthe reaction mixture was concentrated
  3. additiondiluted with methylene chloride
  4. washthe solution was then washed with saturated sodium bicarbonate aqueous solution and saturated brine
  5. dry with materialthe organic layer was dried over magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-07c71cfcc2b64bec8a6a927da5a832e3
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181250B2

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