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Hydrochloric Acid → 3-(5-iodo-1H-indazol-1-yl)benzoic acid

HRID 1098942
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반응식

HRID 1098942 반응식
F[C:2]1[CH:19]=[CH:18][C:17]([I:20])=[CH:16][C:3]=1[CH:4]=[N:5][NH:6][C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][CH:15]=1)[C:10]([OH:12])=[O:11].CC(C)([O-])C.[K+].Cl>CN1C(=O)CCC1.O>[I:20][C:17]1[CH:16]=[C:3]2[C:2](=[CH:19][CH:18]=1)[N:6]([C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][CH:15]=1)[C:10]([OH:12])=[O:11])[N:5]=[CH:4]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 23665647Potassium tert-butoxideHCID 670412113-(2-(2-Fluoro-5-iodobenzylidene)hydrazinyl)benzoic acid

생성물 1

HCID 574320973-(5-iodo-1H-indazol-1-yl)benzoic acid수율 107.4%

시약·촉매·용매 2

HCID 962Water용매HCID 13387
N-methyl-2-pyrrolidone
용매

실험 절차

3-(2-(2-fluoro-5-iodobenzylidene)hydrazinyl)benzoic acid (3.47 g, 9 mmol) and potassium tert. butoxide (2.3 g, 20.5 mmol) was stirred under argon atmosphere in NMP (45 mL) at 150° C. for 30 min. After cooling, the mixture was diluted with water (100 mL), acidified with aqueous HCl (1.7 M) and extracted trice with EtOAc. The combined organic phases were washed twice with water and then with brine. Evaporation of the organic phase afforded crude title compound (3.52 g, quant.) as a light brown, amorphous, gummy solid.

후처리

  1. temperatureAfter cooling
  2. extractionextracted trice with EtOAc
  3. washThe combined organic phases were washed twice with water
  4. customEvaporation of the organic phase

출처 및 근거

ORD 기록
ord-92df082fc27d4a2da25140b3ddd35e65
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08143290B2

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