Dichloromethane ethylacetate → Tert-butyl 4-(2-methyl-3-oxo-3,4-dihydropyrido[2,3-b]pyrazin-8-yloxy)naphthalen-1-ylcarbamate

HRID 1402990

反応式

HRID 1402990 の反応式
[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([O:9][C:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[C:13]([NH:20][C:21](=[O:27])[O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[CH:12][CH:11]=2)[CH:5]=[CH:4][N:3]=1.[CH2:28](Cl)Cl.CCO[C:34]([CH3:36])=[O:35]>CCOC(C)=O.CO>[CH3:28][C:36]1[C:34](=[O:35])[NH:1][C:2]2[N:3]=[CH:4][CH:5]=[C:6]([O:9][C:10]3[C:19]4[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=4)[C:13]([NH:20][C:21](=[O:27])[O:22][C:23]([CH3:24])([CH3:26])[CH3:25])=[CH:12][CH:11]=3)[C:7]=2[N:8]=1

参加物

4

反応物 2

HCID 21226138Dichloromethane ethylacetateHCID 44186229Tert-butyl 4-(2,3-diaminopyridin-4-yloxy)naphthalen-1-ylcarbamate

生成物 1

HCID 46900747Tert-butyl 4-(2-methyl-3-oxo-3,4-dihydropyrido[2,3-b]pyrazin-8-yloxy)naphthalen-1-ylcarbamate

試薬・触媒・溶媒 1

HCID 21584119Ethylacetate methanol溶媒

実験手順

Method D2 was used with tert-butyl 4-(2,3-diaminopyridin-4-yloxy)naphthalen-1-ylcarbamate to afford a mixture of isomers. The residue was chromatographed (eluent: CH2Cl2/EtOAc: 6/1 towards 0/1 then EtOAc/MeOH:95/5) to afford at first tert-butyl 4-(2-methyl-3-oxo-3,4-dihydropyrido[2,3-b]pyrazin-8-yloxy)naphthalen-1-ylcarbamate as a slightly yellow solid (401 mg, 0.958 mmol, 35%) and then tert-butyl 4-(3-methyl-2-oxo-1,2-dihydropyrido[2,3-b]pyrazin-8-yloxy)naphthalen-1-ylcarbamate as a yellow solid (607 mg, 1.45 mmol, 53%).

後処理

  1. customto afford
  2. additiona mixture of isomers
  3. customThe residue was chromatographed (eluent

出典と根拠

ORDレコード
ord-a63950ae0bbb4703b922ae73847376ce
出典データセット
uspto-grants-2014_12
特許番号
US08912191B2

関連ノート

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