Ammonium Acetate → 4-Chloro-6-methyl-2-oxo-1,2-dihydro-quinoline-3-carbonitrile

HRID 1767531ノート

反応式

HRID 1767531 の反応式
C([O-])(=[O:3])C.[NH4+].Cl[C:7]1[C:16]([C:17]#[N:18])=[C:15]([Cl:19])[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([CH3:20])[CH:13]=2)[N:8]=1>C(O)(=O)C>[Cl:19][C:15]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([CH3:20])[CH:13]=2)[NH:8][C:7](=[O:3])[C:16]=1[C:17]#[N:18]

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 210819292,4-Dichloro-6-methylquinoline-3-carbonitrile

生成物 1

HCID 210819634-Chloro-6-methyl-2-oxo-1,2-dihydro-quinoline-3-carbonitrile収率 69%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
140 °C

実験手順

Ammonium acetate was added to a suspension of Compound 105 (7.1 g, 29.95 mmol) in glacial acetic acid and heated at 140° C. for 4 h. The solution was cooled and poured into ice water. The solids formed were filtered, washed by water, and dried under vacuum to yield 4.5 g (69%) of white solids. M.P. 264° C. 1H NMR (DMSO-d6): δ 2.32 (s, 3H), 7.34 (d, J=8.4 Hz, 1H), 7.63 (dd, J=1.5, 8.4 Hz, 1H), 7.75 (s, 1H). EIMS m/z 219 (M+1).

後処理

  1. temperatureThe solution was cooled
  2. customThe solids formed
  3. filtrationwere filtered
  4. washwashed by water
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-f6af3d8a7b4941268102e372f93af2f5
出典データセット
uspto-grants-2007_06
特許番号
US07235546B2

反応ノート

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