Hydrochloric Acid → N4-[4-(tert-Butyl)-1,3-thiazol-2-yl]-2-aminoisonicotinamide

HRID 1828441노트

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HRID 1828441 반응식
[C:1]([C:5]1[N:6]=[C:7]([NH:10][C:11](=[O:22])[C:12]2[CH:17]=[CH:16][N:15]=[C:14]([NH:18]C(=O)C)[CH:13]=2)[S:8][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].Cl>C(O)C>[C:1]([C:5]1[N:6]=[C:7]([NH:10][C:11](=[O:22])[C:12]2[CH:17]=[CH:16][N:15]=[C:14]([NH2:18])[CH:13]=2)[S:8][CH:9]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 22063745N4-[4-(tert-Butyl)-1,3-thiazol-2-yl]-2-(acetylamino)isonicotinamide

생성물 1

HCID 22063525N4-[4-(tert-Butyl)-1,3-thiazol-2-yl]-2-aminoisonicotinamide수율 52.2%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
85 °C

실험 절차

N4-[4-(tert-Butyl)-1,3-thiazol-2-yl]-2-(acetylamino)isonicotinamide (546 mg) dissolved in ethanol (12 ml) was added dropwise with concentrated hydrochloric acid (1.2 ml) at room temperature and stirred at 80-90° C. for 1 hour. The reaction solution was returned to room temperature, concentrated under reduced pressure, neutralized with 1 N sodium hydroxide and extracted with chloroform. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (chloroform→chloroform:methanol=60:1→20:1) to obtain 247.2 mg (52%) of the title compound as white crystals.

후처리

  1. customwas returned to room temperature
  2. concentrationconcentrated under reduced pressure
  3. extractionextracted with chloroform
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customthe resulting residue was purified by silica gel column chromatography (chloroform→chloroform:methanol=60:1→20:1)

출처 및 근거

ORD 기록
ord-a4174dac4bad4b44b79eb207637c13c5
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07056917B2

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