Dimethylformamide → HCID 86667368, 화합물

HRID 334150노트

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HRID 334150 반응식
CNC([C:5]1[NH:6][C:7]2[C:12]([N:13]=1)=[C:11]([N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)[N:10]=[C:9]([Cl:20])[N:8]=2)=O.[C:21](=O)([O-])[O-].[Cs+].[Cs+].[CH3:27][N:28]([CH:30]=[O:31])[CH3:29]>O>[Cl:20][C:9]1[N:10]=[C:11]([N:14]2[CH2:15][CH2:16][O:17][CH2:18][CH2:19]2)[C:12]2[N:13]=[C:5]3[N:6]([C:7]=2[N:8]=1)[CH2:21][CH2:27][N:28]([CH3:29])[C:30]3=[O:31]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 10796Cesium carbonateHCID 178485563HCID 178485563, 화합물

생성물 1

HCID 86667368HCID 86667368, 화합물수율 77%

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

A mixture of 2-chloro-6-morpholin-4-yl-9H-purine-8-carboxylic acid methylamide (56 mg, 0.19 mmol) 1,2-dibromoethane (0.058 mL, 0.68 mmol) and cesium carbonate (0.25 g, 0.76 mmol) in DMF (2 mL) was heated at 100° C. for 2 h, then cooled, diluted with water and extracted five times with ethyl acetate. The combined extracts were dried (Na2SO4) and concentrated in vacuo. The resulting residue was triturated twice with diethyl ether and the solid was dried under vacuum to give 3-Chloro-7-methyl-1-morpholin-4-yl-6,7-dihydro-5H-2,4,4b,7,9-pentaaza-fluoren-8-one (47 mg, 77%). LCMS RT=2.36, [M+H]+=323/32

후처리

  1. temperaturecooled
  2. extractionextracted five times with ethyl acetate
  3. dry with materialThe combined extracts were dried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. customThe resulting residue was triturated twice with diethyl ether
  6. customthe solid was dried under vacuum

출처 및 근거

ORD 기록
ord-8f559a29159f4a94bfa4beccf6228985
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883799B2

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