Hydrazine hydrate (1:1) → HCID 178507276, 화합물

HRID 347997

반응식

HRID 347997 반응식
[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[C:4]([CH2:6][C:7]#[N:8])=O.O.[NH2:14][NH2:15]>C(O)C>[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[C:4]1[CH:6]=[C:7]([NH2:8])[NH:14][N:15]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 27342012-Chlorobenzoylacetonitrile

생성물 1

HCID 178507276HCID 178507276, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 2-chlorobenzoylacetonitrile (15.9 g, 89 mmol) and hydrazine hydrate (8.9 g, 0.18 mol) in ethanol (2 ml) was heated at reflux for 22 hr. After cooling to room temperature, the reaction was concentrated, in vacuo. The residue was dissolved in ethyl acetate, washed with water and brine, dried (MgSO4), and concentrated, in vacuo, to a brown oil. Flash chromatography using 10% ethyl acetate in methylene chloride, changing to 5% methanol in methylene chloride as eluant afforded title product I-1A-1a (17.3 g, quantitative): +ESI MS (M+1) 194.2; 1H NMR (400 MHz, CD3OD) δ 7.60–7.25 (m, 4H), 5.99 (br s, 1H).

후처리

  1. temperatureat reflux for 22 hr
  2. concentrationthe reaction was concentrated, in vacuo
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water and brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated, in vacuo, to a brown oil

출처 및 근거

ORD 기록
ord-a23ee3c3ff084847b808711a4f6189ce
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176210B2

연결된 노트

불러오는 중…