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Hydrazine hydrate (1:1) → HCID 21332725、化合物

HRID 1629971
ノート
印刷プレビュー

反応式

HRID 1629971 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 21332725HCID 21332725、化合物収率 95.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-229cdc57d4a5460b8590adb6594a944a
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08791114B2

反応ノート

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