(E)-3-Dimethylamino-1-phenyl-propenone → HCID 86725497、化合物

HRID 878518ノート

反応式

HRID 878518 の反応式
[NH:1]([C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][N:10]=1)[C:6]#[N:7])[NH2:2].CN(C)/[CH:13]=[CH:14]/[C:15]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=O>C(O)C.CC(O)=O>[C:17]1([C:15]2[N:1]([C:3]3[CH:4]=[C:5]([CH:8]=[CH:9][N:10]=3)[C:6]#[N:7])[N:2]=[CH:13][CH:14]=2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

5

反応物 2

HCID 5398495(E)-3-Dimethylamino-1-phenyl-propenoneHCID 201187142-Hydrazinylpyridine-4-carbonitrile

生成物 1

HCID 86725497HCID 86725497、化合物収率 81.2%

試薬・触媒・溶媒 2

HCID 176Acetic Acid触媒HCID 702Ethanol溶媒

実験手順

To a solution of 2-hydrazinylisonicotinonitrile (100 mg, 0.75 mmol, 1.0 eq., PREPARATION 2) and (E)-3-(dimethylamino)-1-phenylprop-2-en-1-one (132 mg, 0.75 mmol, 1.0 eq.) in ethanol (10 mL) was added 2-5 drops of AcOH. The reaction mixture was under reflux conditions for 12 h. After reaction completion, volatiles were removed under reduced pressure, and the resultant crude material was purified by flash column chromatography (20% EtOAc/hexane) to obtain the title compound as a yellow oil (150 mg, 81% yield). [M+H] Calc'd for C15H10N4, 247.09; Found 247.

後処理

  1. customAfter reaction completion, volatiles
  2. customwere removed under reduced pressure
  3. customthe resultant crude material was purified by flash column chromatography (20% EtOAc/hexane)

出典と根拠

ORDレコード
ord-40ab2788f5cb46009cafb0e8377bad39
出典データセット
uspto-grants-2015_03
特許番号
US08987461B2

反応ノート

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