Acetophenone → Acetophenone benzoylhydrazone

HRID 22098

反応式

HRID 22098 の反応式
[C:1]([NH:9][NH2:10])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:11]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)(=O)[CH3:12]>O1CCCC1>[C:1]([NH:9][N:10]=[C:11]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:12])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 7410AcetophenoneHCID 11955Benzoylhydrazine

生成物 1

HCID 346107Acetophenone benzoylhydrazone

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
25 °C

実験手順

To a solution of benzoic acid hydrazide (5.70 g, 0.042 mol) in tetrahydrofuran (75 mL) was added acetophenone (5.5 g, 0.046 mol) followed by concentrated. HCl (3 drops). The reaction was allowed to stir for 12 h at 25° C. during which time the product precipitated as a colorless crystalline solid. The product was filtered, washed with tetrahydrofuran (1×30 mL), diethyl ether (3×60 mL) and pentane (2×60 mL), and the crystalline solids were dried in vacuo (6.65 g, 64%). 1H NMR (CD2Cl2): δ2.35 (s, 3H, CH3), 7.30-8.0 (m, 10H, Ph), 9.0 (br, 1H, NH). All other substrates were prepared in a similar fashion.

後処理

  1. concentrationby concentrated
  2. customprecipitated as a colorless crystalline solid
  3. filtrationThe product was filtered
  4. washwashed with tetrahydrofuran (1×30 mL), diethyl ether (3×60 mL) and pentane (2×60 mL)
  5. customthe crystalline solids were dried in vacuo (6.65 g, 64%)
  6. customAll other substrates were prepared in a similar fashion

出典と根拠

ORDレコード
ord-0b866c1b184048648795054c228cf6bd
出典データセット
uspto-grants-1995_06
特許番号
US05426223

関連ノート

読み込み中…