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Methyl 1-(Aminomethyl)cyclobutanecarboxylate → 1-{[(1-Cyano-4-hydroxy-7-phenoxy-isoquinoline-3-carbonyl)-amino]-methyl}-cyclobutanecarboxylic acid methyl ester

HRID 1480947
ノート
印刷プレビュー

反応式

HRID 1480947 の反応式
CO[C:3]([C:5]1[N:6]=[C:7]([C:23]#[N:24])[C:8]2[C:13]([C:14]=1[OH:15])=[CH:12][CH:11]=[C:10]([O:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[CH:9]=2)=[O:4].[CH3:25][O:26][C:27]([C:29]1([CH2:33][NH2:34])[CH2:32][CH2:31][CH2:30]1)=[O:28]>CO>[CH3:25][O:26][C:27]([C:29]1([CH2:33][NH:34][C:3]([C:5]2[N:6]=[C:7]([C:23]#[N:24])[C:8]3[C:13]([C:14]=2[OH:15])=[CH:12][CH:11]=[C:10]([O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:9]=3)=[O:4])[CH2:32][CH2:31][CH2:30]1)=[O:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 25918829Methyl 1-(Aminomethyl)cyclobutanecarboxylateHCID 89812860Methyl 1-cyano-4-hydroxy-7-phenoxyisoquinoline-3-carboxylate

生成物 1

HCID 898129681-{[(1-Cyano-4-hydroxy-7-phenoxy-isoquinoline-3-carbonyl)-amino]-methyl}-cyclobutanecarboxylic acid methyl ester

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

After a mixture of 1-cyano-4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (129 mg, 0.401 mmol), 1-aminomethyl-cyclobutanecarboxylic acid methyl ester (115 mg, 0.803 mmol in MeOH was microwaved at 150° C. for 500 min; cooled, concentrated, the residue was partitioned between EtOAc and diluted HCl solution, EtOAc phase was washed with water and diluted NaCl solution, dried over anhydrous sodium sulfate, filtered, concentrated and column purified to give product (172 mg). LC MS ESI+: 432 (M+1)+.

後処理

  1. customwas microwaved at 150° C. for 500 min
  2. temperaturecooled
  3. concentrationconcentrated
  4. customthe residue was partitioned between EtOAc and diluted HCl solution, EtOAc phase
  5. washwas washed with water and diluted NaCl solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customcolumn purified

出典と根拠

ORDレコード
ord-22c94f61ee944e43bd8fad31c8fdc65c
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09409892B2

反応ノート

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