Methanol → HCID 89812870、化合物

HRID 1481226ノート

反応式

HRID 1481226 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].Cl.Cl.[CH2:27]([O:29][C:30](=[O:40])[CH2:31][C@@H:32]([NH2:39])[C:33]1[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=1)C.C[O-].[Na+].CO>>[CH3:27][O:29][C:30](=[O:40])[CH2:31][C@@H:32]([NH:39][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:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)[CH:9]=2)=[O:4])[C:33]1[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=1

参加物

5

反応物 4

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 44890919Ethyl (3R)-3-amino-3-(pyridin-3-yl)propanoate--hydrogen chloride (1/2)HCID 89812860Methyl 1-cyano-4-hydroxy-7-phenoxyisoquinoline-3-carboxylate

生成物 1

HCID 89812870HCID 89812870、化合物収率 67%

反応条件

温度
140 °C

実験手順

1-Cyano-4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (50 mg, 0.156 mmol) was combined in a CEM microwave tube (10 mL) with (R)-3-amino-3-pyridin-3-yl-propionic acid ethyl ester dihydrochloride (134 mg, 0.5 mmol) (commercially available from AstaTech 46345) and a solution of sodium methoxide in methanol (2 mL, 0.5M, 1 mmol) was added with stirring. The reaction was heated to 140° C. in the CEM microwave apparatus for approximately 90 minutes. The reaction was cooled, concentrated under vacuum and filtered through silica to provide 49 mg of the desired product which was used without additional purification.

後処理

  1. additionwas added
  2. temperatureThe reaction was cooled
  3. concentrationconcentrated under vacuum
  4. filtrationfiltered through silica

出典と根拠

ORDレコード
ord-d8308ff37e954e1a9a34dbe8965b2fbb
出典データセット
uspto-grants-2016_08
特許番号
US09409892B2

反応ノート

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