Triethylamine → 4D-083

HRID 1995343ノート

反応式

HRID 1995343 の反応式
[O:1]=[C:2]1[C:7]([C:8](O)=[O:9])=[CH:6][C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:4][NH:3]1.C([N:19](CC)CC)C>ClCCl>[O:1]=[C:2]1[C:7]([C:8]([NH2:19])=[O:9])=[CH:6][C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:4][NH:3]1

参加物

4

反応物 2

HCID 8471TriethylamineHCID 121489343-Oxo-6-phenyl-2,3-dihydropyridazine-4-carboxylic acid

生成物 1

HCID 14753284D-083

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarboxylic acid (1.92 g) ethyl chloroformate (1.1 g) and triethylamine (2.0 ml) in 50 ml of dichloromethane is allowed to stir at 25°-30° C. for 2 hours. Ammonia gas is then bubbled into the mixture for 15 minutes. Water (50 ml) is added and the dichloromethane is separated and concentrated on the rotary evaporator. The residue is chromatographed on silica gel with 2% methanol and chloroform to give 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarboxamide.

後処理

  1. customAmmonia gas is then bubbled into the mixture for 15 minutes
  2. additionWater (50 ml) is added
  3. customthe dichloromethane is separated
  4. concentrationconcentrated on the rotary evaporator
  5. customThe residue is chromatographed on silica gel with 2% methanol and chloroform

出典と根拠

ORDレコード
ord-6d64a749ca7c42b59c90b51c53f1cb0b
出典データセット
uspto-grants-1983_09
特許番号
US04404203

反応ノート

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