Hydrazine hydrate (1:1) → HCID 178507276、化合物

HRID 347997

反応式

HRID 347997 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 178507276HCID 178507276、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a23ee3c3ff084847b808711a4f6189ce
出典データセット
uspto-grants-2007_02
特許番号
US07176210B2

関連ノート

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