Dimethylformamide → HCID 86641478, 화합물

HRID 472763노트

반응식

HRID 472763 반응식
[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]

참가 물질

6

반응물 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

생성물 1

HCID 86641478HCID 86641478, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e2e36f995c604bd7b5ba6f6133d436be
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633211B2

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