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

HRID 1280407노트

반응식

HRID 1280407 반응식
[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]

참가 물질

5

반응물 3

HCID 120273N-Iodosuccinimide2회HCID 516892Sodium BicarbonateHCID 225623382-(4-ethoxy-phenyl)-pyrazolo[1,5-b]pyridazine-3-carboxylic Acid

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-3147a330d70d40f48335bb7db4958a53
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06451794B1

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