N-Iodosuccinimide → 2-(4-Ethoxy-phenyl)-3-iodo-pyrazolo[1,5-b]pyridazine

HRID 1280407ノート

反応式

HRID 1280407 の反応式
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:18](C(O)=O)=[C:17]3[N:12]([N:13]=[CH:14][CH:15]=[CH:16]3)[N:11]=2)=[CH:6][CH:5]=1)[CH3:2].[I:22]N1C(=O)CCC1=O.C(=O)(O)[O-].[Na+]>CN(C=O)C>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:18]([I:22])=[C:17]3[N:12]([N:13]=[CH:14][CH:15]=[CH:16]3)[N:11]=2)=[CH:6][CH:5]=1)[CH3:2]

参加物

5

反応物 3

HCID 120273N-Iodosuccinimide2 回HCID 516892Sodium BicarbonateHCID 225623382-(4-ethoxy-phenyl)-pyrazolo[1,5-b]pyridazine-3-carboxylic Acid

生成物 1

HCID 225623392-(4-Ethoxy-phenyl)-3-iodo-pyrazolo[1,5-b]pyridazine収率 47%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2-(4-ethoxy-phenyl)-pyrazolo[1,5-b]pyridazine-3-carboxylic acid (710 mg), N-iodosuccinimide (678 mg) and sodium bicarbonate (717 mg) in DMF (8 ml) was stirred for 4 h. A further quantity of N-iodosuccinimide (100 mg) was added and stirring continued for 2 h. Aqueous workup gave a dark brown solid which was purified by SPE with dichloromethane as eluant. This gave the title compound as an orange-brown solid (429 mg, 47%).

後処理

  1. stirringstirring
  2. waitcontinued for 2 h
  3. customAqueous workup gave a dark brown solid which
  4. customwas purified by SPE with dichloromethane as eluant

出典と根拠

ORDレコード
ord-3147a330d70d40f48335bb7db4958a53
出典データセット
uspto-grants-2002_09
特許番号
US06451794B1

反応ノート

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