Hydrazine hydrate (1:1) → HCID 178420101、化合物

HRID 530297ノート

反応式

HRID 530297 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 178420101HCID 178420101、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-6ff3111c2d6d4b42bc3cff12ae976913
出典データセット
uspto-grants-2016_05
特許番号
US09353082B2

反応ノート

読み込み中…