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Ethyl Acetate → HCID 19089105, 화합물

HRID 1463977
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HRID 1463977 반응식
[CH2:1]([O:3][CH:4]([O:8][CH2:9][CH3:10])[CH2:5][NH:6][NH2:7])[CH3:2].CO[C:13](=[CH2:16])[C:14]#[N:15].C(OCC)(=O)C>O>[CH2:1]([O:3][CH:4]([O:8][CH2:9][CH3:10])[CH2:5][N:6]1[C:14]([NH2:15])=[CH:13][CH:16]=[N:7]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 322952(2,2-Diethoxyethyl)hydrazineHCID 132442492-Methoxyprop-2-enenitrile

생성물 1

HCID 19089105HCID 19089105, 화합물수율 19.3%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A mixture of hydrazinoacetaldehyde diethyl acetal (21 g) and methoxyacrylonitrile (11.8 g) in water (150 ml) was refluxed for 2 days. After the reaction mixture was cooled, to the mixture was added a mixture of water and ethyl acetate. The separated organic layer was washed with brine and dried over magnesium sulfate. The solvent was evaporated and the residue was subjected to column chromatography on silica gel using ethyl acetate as an eluent. Fractions containing the object compound were combined and evaporated to give 1-(2,2-diethoxyethyl)-5-aminopyrazole (5.45 g).

후처리

  1. temperaturewas refluxed for 2 days
  2. temperatureAfter the reaction mixture was cooled, to the mixture
  3. additionwas added
  4. washThe separated organic layer was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated
  7. additionFractions containing the object compound
  8. customevaporated

출처 및 근거

ORD 기록
ord-18a4391a669a48c38274b7f29de18659
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05302712

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