(E)-3-Dimethylamino-1-phenyl-propenone → HCID 86725497, 화합물

HRID 514361노트

반응식

HRID 514361 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 86725497HCID 86725497, 화합물수율 81.2%

시약·촉매·용매 2

HCID 176Acetic Acid촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d87a3fedad8e4006888bcc9599d38f29
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09107916B2

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