Hydrazine hydrate (1:1) → HCID 178420101, 화합물

HRID 530297노트

반응식

HRID 530297 반응식
C[N:2](C)/[CH:3]=[CH:4]/[C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=O.O.[NH2:15]N>C(O)C>[C:7]1([C:5]2[CH:4]=[CH:3][NH:2][N:15]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 5398495(E)-3-Dimethylamino-1-phenyl-propenone

생성물 1

HCID 178420101HCID 178420101, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
100 °C

실험 절차

To a stirred solution of (E)-3-(dimethylamino)-1-phenylprop-2-en-1-one (2.63 g, 15 mmol) in ethanol (40 ml) was added hydrazine hydrate (1.459 ml, 30.0 mmol). The reaction was heated to 100° C. for 2 hours. Whereupon was cooled to room temperature and ethanol was removed by vacuum. The residue was partitioned between DCM and water. The organic phase was dried over MgSO4 and filtered. After evaporation the crude product was purified by triturating with a mixture of petroleumether and ethyl acetate. (Yield: 1.59 g, 73%).

후처리

  1. temperatureWhereupon was cooled to room temperature
  2. customethanol was removed by vacuum
  3. customThe residue was partitioned between DCM and water
  4. dry with materialThe organic phase was dried over MgSO4
  5. filtrationfiltered
  6. customAfter evaporation the crude product
  7. customwas purified
  8. customby triturating with a mixture of petroleumether and ethyl acetate

출처 및 근거

ORD 기록
ord-6ff3111c2d6d4b42bc3cff12ae976913
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353082B2

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