Potassium Carbonate → HCID 117666963, 화합물

HRID 1526253노트

반응식

HRID 1526253 반응식
Cl[C:2]1[N:3]=[C:4]([NH:15][C:16]2[CH:17]=[N:18][N:19]([CH2:21][CH2:22][OH:23])[CH:20]=2)[C:5]([C:12]([NH2:14])=[O:13])=[N:6][C:7]=1[C:8]([OH:11])([CH3:10])[CH3:9].[NH2:24][C:25]1[CH:26]=[CH:27][C:28]([F:32])=[C:29]([OH:31])[CH:30]=1.C(=O)([O-])[O-].[K+].[K+].[Cl-].[Na+].O.O>CN1CCCC1=O>[NH2:24][C:25]1[CH:26]=[CH:27][C:28]([F:32])=[C:29]([CH:30]=1)[O:31][C:2]1[N:3]=[C:4]([NH:15][C:16]2[CH:17]=[N:18][N:19]([CH2:21][CH2:22][OH:23])[CH:20]=2)[C:5]([C:12]([NH2:14])=[O:13])=[N:6][C:7]=1[C:8]([OH:11])([CH3:10])[CH3:9]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 226414135-Amino-2-fluorophenolHCID 23713072Sodium chloride dihydrateHCID 117667243HCID 117667243, 화합물

생성물 1

HCID 117666963HCID 117666963, 화합물수율 52.3%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

A mixture of 5-chloro-3-{[1-(2-hydroxyethyl)-1H-pyrazol-4-yl]amino}-6-(2-hydroxypropan-2-yl)pyrazine-2-carboxamide (790 mg), 5-amino-2-fluorophenol (442 mg), potassium carbonate (641 mg), and N-methylpyrrolidone (8 mL) was reacted at 100° C. for 2 hours. To the reactant was added a mixed solution of saturated brine:water (1:1), followed by extraction with ethyl acetate. The organic phase was dried over anhydrous sodium sulfate and then the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (eluent; chloroform:methanol=99:1-80:20) to obtain 5-(5-amino-2-fluorophenoxy)-3-{[1-(2-hydroxyethyl)-1H-pyrazol-4-yl]amino}-6-(2-hydroxypropan-2-yl)pyrazine-2-carboxamide (523 mg) as a pale brown solid.

후처리

  1. customwas reacted at 100° C. for 2 hours
  2. extractionfollowed by extraction with ethyl acetate
  3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography (eluent; chloroform:methanol=99:1-80:20)

출처 및 근거

ORD 기록
ord-3134322645914a5fbc3a9a8c44ceab07
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085540B2

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