Dimethylformamide → HCID 86667368、化合物

HRID 334150ノート

反応式

HRID 334150 の反応式
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]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 10796Cesium carbonateHCID 178485563HCID 178485563、化合物

生成物 1

HCID 86667368HCID 86667368、化合物収率 77%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-8f559a29159f4a94bfa4beccf6228985
出典データセット
uspto-grants-2014_11
特許番号
US08883799B2

反応ノート

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