Ethanol → HCID 178509693, 화합물

HRID 1501428노트

반응식

HRID 1501428 반응식
C[N:2](C)/[CH:3]=[CH:4]/[C:5]([C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][CH:14]=1)[C:10]#[N:11])=O.C(O)C.[NH2:19]N>>[NH:2]1[CH:3]=[CH:4][C:5]([C:7]2[CH:8]=[C:9]([CH:12]=[CH:13][CH:14]=2)[C:10]#[N:11])=[N:19]1

참가 물질

4

반응물 3

HCID 702EthanolHCID 9321HydrazineHCID 57140731-(3-Cyanophenyl)-3-(dimethylamino)acrolein

생성물 1

HCID 178509693HCID 178509693, 화합물수율 84.7%

실험 절차

The 3-[(2E)-3-(dimethylamino)prop-2-enoyl]benzonitrile (0.600 g, 0.00300 mol) was dissolved in ethanol (20.0 mL, 0.342 mol) and hydrazine (0.56 mL, 0.018 mol) under an atmosphere of nitrogen was stirred at room temperature for 1.5 h. The reaction was concentrated in vacuo to give a dark product which was purified by FCC on silica gel, eluting with ethyl acetate-hexane 1:1 to give 3-(1H-pyrazol-3-yl)benzonitrile as an oil (0.430 g, 84%), LC/MS (M+H)+: 170.

후처리

  1. concentrationThe reaction was concentrated in vacuo
  2. customto give a dark product which
  3. customwas purified by FCC on silica gel
  4. washeluting with ethyl acetate-hexane 1:1

출처 및 근거

ORD 기록
ord-3c75800d635b499d806bf7565923a01c
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206187B2

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