Hydrazinecarboxylic acid, ethyl ester → Ethyl 3-[6-(p-bromophenyl)-5-methyl-3-pyridazinyl]carbazate

HRID 372708ノート

反応式

HRID 372708 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11](Cl)=[CH:10][C:9]=2[CH3:15])=[CH:4][CH:3]=1.[C:16]([O:20][CH2:21][CH3:22])(=[O:19])[NH:17][NH2:18]>C(O)CCC>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([NH:18][NH:17][C:16]([O:20][CH2:21][CH3:22])=[O:19])=[CH:10][C:9]=2[CH3:15])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 203982893-(p-Bromophenyl)-6-chloro-4-methylpyridazine

生成物 1

HCID 20326503Ethyl 3-[6-(p-bromophenyl)-5-methyl-3-pyridazinyl]carbazate

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A mixture of 8.49 g. of 6-(p-bromophenyl)-5-methyl-3-chloropyridazine and 6.25 g. of ethyl carbazate in 100 ml. of n-butyl alcohol is prepared. This solution is stirred and heated at reflux temperature for 4 hours. The reaction mixture is cooled to room temperature and the solvent removed on a rotating evaporator. Water is added to the residue and the resulting solid filtered, washed with water, ether and dried. The product is recrystallized from ethanol to yield the product, m.p. 178°-179° C.

後処理

  1. additionA mixture of 8.49 g
  2. temperatureheated
  3. temperatureat reflux temperature for 4 hours
  4. customthe solvent removed on a rotating evaporator
  5. additionWater is added to the residue
  6. filtrationthe resulting solid filtered
  7. washwashed with water, ether
  8. customdried
  9. customThe product is recrystallized from ethanol
  10. customto yield the product, m.p. 178°-179° C.

出典と根拠

ORDレコード
ord-f8433282216e4f7facc71cd93ed17452
出典データセット
uspto-grants-1978_05
特許番号
US04092311

反応ノート

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