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Hydrochloric Acid → 3-(2-methylpyridin-4-yl)-1-trityl-1H-indazole-5-carboxylic acid

HRID 1467313
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인쇄 미리보기

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HRID 1467313 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:17]([O:19]CC)=[O:18])[CH:15]=3)[N:10]([C:22]([C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[N:9]=2)[CH:5]=[CH:4][N:3]=1.CO.[OH-].[Na+].Cl>C(O)(C)C.C(Cl)(Cl)Cl>[CH3:1][C:2]1[CH:7]=[C:6]([C:8]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:17]([OH:19])=[O:18])[CH:15]=3)[N:10]([C:22]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)([C:35]3[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=3)[C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[N:9]=2)[CH:5]=[CH:4][N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 67984978ethyl 3-(2-methylpyridin-4-yl)-1-trityl-1H-indazole-5-carboxylate

생성물 1

HCID 679849753-(2-methylpyridin-4-yl)-1-trityl-1H-indazole-5-carboxylic acid수율 98.6%

시약·촉매·용매 2

HCID 3776
Isopropanol
용매
HCID 6212Chloroform용매

반응 조건

온도
80 °C

실험 절차

In a sealed flask was added ethyl 3-(2-methylpyridin-4-yl)-1-trityl-1H-indazole-5-carboxylate (420 mg, 0.802 mmol), MeOH (6 ml), and sodium hydroxide (1N in water, 4 ml, 4.00 mmol). The resulting mixture was then heated for 60 min at a temperature of 80° C. with stirring. The mixture was then neutralized with HCl (2N in water), diluted with 10% isopropanol in chloroform, washed with water, dried with sodium sulfate, filtered, and concentrated to afford 3-(2-methylpyridin-4-yl)-1-trityl-1H-indazole-5-carboxylic acid (392 mg, 0.791 mmol) as a light yellow solid. The crude product was progressed to the next step without purification.

후처리

  1. washwashed with water
  2. dry with materialdried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7fe3d1c8fcca471b8d6273e8759085f1
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08999957B2

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