Dimethylformamide → HCID 86641478、化合物

HRID 472763ノート

反応式

HRID 472763 の反応式
[C:1]([O:5][C:6](=[O:21])[CH2:7][N:8]1[C:13](=[O:14])[C:12]2[C:15]([Cl:19])=[N:16][CH:17]=[CH:18][C:11]=2[NH:10][C:9]1=[O:20])([CH3:4])([CH3:3])[CH3:2].Br[CH2:23][C:24]([NH:26][C:27]1[CH:32]=[C:31]([Cl:33])[C:30]([O:34][CH3:35])=[CH:29][C:28]=1[O:36][CH3:37])=[O:25].C([O-])([O-])=O.[Cs+].[Cs+].CN(C=O)C>O>[C:1]([O:5][C:6](=[O:21])[CH2:7][N:8]1[C:13](=[O:14])[C:12]2[C:15]([Cl:19])=[N:16][CH:17]=[CH:18][C:11]=2[N:10]([CH2:23][C:24](=[O:25])[NH:26][C:27]2[CH:32]=[C:31]([Cl:33])[C:30]([O:34][CH3:35])=[CH:29][C:28]=2[O:36][CH3:37])[C:9]1=[O:20])([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 10796Cesium carbonateHCID 636790772-Bromo-N-(5-chloro-2,4-dimethoxy-phenyl)-acetamideHCID 86641480(5-Chloro-2,4-dioxo-1,4-dihydro-2H-pyrido[4,3-d]pyrimidin-3-yl)-acetic acid tert-butyl ester

生成物 1

HCID 86641478HCID 86641478、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A vial is charged with (5-Chloro-2,4-dioxo-1,4-dihydro-2H-pyrido[4,3-d]pyrimidin-3-yl)-acetic acid tert-butyl ester (53.1 mg, 0.17 mmol), 2-Bromo-N-(5-chloro-2,4-dimethoxy-phenyl)-acetamide (58.1 mg, 0.187 mmol), and Cs2CO3 (124.3 mg, 0.34 mmol). The mixture is treated with DMF (3 ml) and the solution stirred at RT overnight. The reaction mixture is treated with water and the product extracted with EtOAc (3×10 ml). The organic extracts are combined and washed with water (2×10 ml), dried (MgSO4), filtered and concentrated in vacuo. The crude material is purified using flash column chromatography with an eluent system of isohexane:EtOAc to give the title compound; [M+H]+ 539.

後処理

  1. extractionthe product extracted with EtOAc (3×10 ml)
  2. washwashed with water (2×10 ml)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude material is purified

出典と根拠

ORDレコード
ord-e2e36f995c604bd7b5ba6f6133d436be
出典データセット
uspto-grants-2014_01
特許番号
US08633211B2

反応ノート

読み込み中…