Potassium Carbonate → HCID 117666963、化合物

HRID 1526253ノート

反応式

HRID 1526253 の反応式
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]

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 226414135-Amino-2-fluorophenolHCID 23713072Sodium chloride dihydrateHCID 117667243HCID 117667243、化合物

生成物 1

HCID 117666963HCID 117666963、化合物収率 52.3%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-3134322645914a5fbc3a9a8c44ceab07
出典データセット
uspto-grants-2015_07
特許番号
US09085540B2

反応ノート

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