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Hydrazine hydrate (1:1) → HCID 21332725, 화합물

HRID 1629971
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반응식

HRID 1629971 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11](=O)[CH2:12][CH2:13][N:14](C)C)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].O.[NH2:19]N>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[CH2:12][CH2:13][NH:14][N:19]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 2118641-(3,4-Dimethoxyphenyl)-3-(dimethylamino)propan-1-one

생성물 1

HCID 21332725HCID 21332725, 화합물수율 95.4%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

To a stirred solution of 1-(3,4-dimethoxyphenyl-3-(dimethylamino)propan-1-one (2.9 g, 0.0122 moles, 1 equiv.) in absolute ethanol was added hydrazine hydrate (99%-100%) (1.18 ml, 0.0244 moles, 2 equiv) drop wise. After that the reaction mixture was refluxed for 4 h at 80° C. under inert atmosphere. Consumption of starting materials was confirmed by LC-MS analysis and TLC. Ethanol and excess hydrazine hydrate was evaporated under reduced pressure and to the crude product was stirred with diethyl ether at RT for 30 mins, filtered washed with ether and finally dried under vacuum to get 2.4 g (95% yield) of the title product as yellow solid.

후처리

  1. customConsumption of starting materials
  2. customEthanol and excess hydrazine hydrate was evaporated under reduced pressure and to the crude product
  3. filtrationfiltered
  4. washwashed with ether
  5. customfinally dried under vacuum

출처 및 근거

ORD 기록
ord-229cdc57d4a5460b8590adb6594a944a
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08791114B2

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