2-Methoxyethanol → 6-Chloro-4-(2-methoxyethoxy)pyrido[3,2-d]pyrimidin-2-amine

HRID 1099105ノート

反応式

HRID 1099105 の反応式
CC(C)([O-])C.[K+].[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[N:12]=[C:13]([NH2:23])[N:14]=[C:15](N3C=NC=N3)[C:16]=2[N:17]=1.[CH3:24][O:25][CH2:26][CH2:27][OH:28]>C(Cl)Cl>[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[N:12]=[C:13]([NH2:23])[N:14]=[C:15]([O:28][CH2:27][CH2:26][O:25][CH3:24])[C:16]=2[N:17]=1

参加物

5

反応物 3

HCID 80192-MethoxyethanolHCID 23665647Potassium tert-butoxideHCID 576983146-Chloro-4-(1H-1,2,4-triazol-1-yl)pyrido[3,2-d]pyrimidin-2-amine

生成物 1

HCID 576983626-Chloro-4-(2-methoxyethoxy)pyrido[3,2-d]pyrimidin-2-amine収率 90%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Potassium tert-butoxide (4 mL; 1M in THF) was added to a suspension mixture of 6-chloro-4-[1,2,4]triazol-1-yl-pyrido[3,2-d]pyrimidin-2-ylamine (1 g) and 2-methoxyethanol (0.32 mL) in DCM (50 mL). After stirring at room temperature for 10 minutes, the mixture was diluted with DCM (100 mL) and washed with brine. The organic layer was dried over Na2SO4 and concentrated to afford 6-chloro-4-(2-methoxy-ethoxy)-pyrido[3,2-d]pyrimidin-2-ylamine as a beige solid (0.91 g, yield: 90%) which was characterized by its mass spectrum as follows: MS (m/z) 225.0 [M+H]+.

後処理

  1. washwashed with brine
  2. dry with materialThe organic layer was dried over Na2SO4
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-0878a950690249b48b7f47dbec8b1e8d
出典データセット
uspto-grants-2012_03
特許番号
US08143394B2

反応ノート

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