Triethylamine → 4D-083

HRID 1995344ノート

反応式

HRID 1995344 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.S(Cl)(Cl)=O>O1CCCC1>[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

5

反応物 3

HCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 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 8028Tetrahydrofuran溶媒

実験手順

In an alternate procedure, a mixture of 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarboxylic acid (1.92 g), triethylamine (3.0 ml), and thionyl chloride (5.0 ml) in tetrahydrofuran is allowed to stir at 20°-25° C. for 6 hours. The mixture is concentrated on the rotary evaporator and the residue is treated with 50 ml of cold ammonium hydroxide solution. The solid product is collected and recrystallized from acetic acid to give 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarboxamide.

後処理

  1. concentrationThe mixture is concentrated on the rotary evaporator
  2. additionthe residue is treated with 50 ml of cold ammonium hydroxide solution
  3. customThe solid product is collected
  4. customrecrystallized from acetic acid

出典と根拠

ORDレコード
ord-091ee31fa94a4af29767edc1a3780f19
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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