Water → 2-benzyl-4,5-dibromopyridazin-3(2H)-one

HRID 612399ノート

反応式

HRID 612399 の反応式
[C:1](O)(=O)/[C:2](=[C:4](\[CH:6]=[O:7])/[Br:5])/[Br:3].Cl.Cl.[CH2:12]([NH:19][NH2:20])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.O>C(O)C>[CH2:12]([N:19]1[C:6](=[O:7])[C:4]([Br:5])=[C:2]([Br:3])[CH:1]=[N:20]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 962WaterHCID 146540Benzylhydrazine dihydrochlorideHCID 3033972Mucobromic Acid

生成物 1

HCID 99026992-benzyl-4,5-dibromopyridazin-3(2H)-one収率 54.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Alternatively, a suspension of mucobromic acid (80 g., 310 mmol.) and benzylhydrazine dihydrochloride (60 g., 310 mmol.) in ethanol was heated to reflux for 16 hours. It was cooled to r.t. and under vigourous stirring water (50 mL) was added. The suspension was cooled in an ice bath and then filtered. The solid was washed with 95% aqueous ethanol and air dried. It was swished in hexanes (200 mL) and diethyl ether (25 mL), filtered and air dried to yield the title compound(58 g.).

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 16 hours
  3. additionwas added
  4. temperatureThe suspension was cooled in an ice bath
  5. filtrationfiltered
  6. washThe solid was washed with 95% aqueous ethanol and air
  7. customdried
  8. filtrationdiethyl ether (25 mL), filtered
  9. customair dried

出典と根拠

ORDレコード
ord-21e0d7d408fb4ae98056a12957933a83
出典データセット
uspto-grants-1999_12
特許番号
US06004960

反応ノート

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