Dimethylamine → HCID 23020406、化合物

HRID 747164ノート

反応式

HRID 747164 の反応式
F[C:2]1[CH:7]=[C:6]([C:8]2[C:9]([C:20]3[O:21][CH:22]=[CH:23][CH:24]=3)=[N:10][C:11]([NH2:19])=[N:12][C:13]=2[C:14]2[O:15][CH:16]=[CH:17][CH:18]=2)[CH:5]=[CH:4][N:3]=1.[CH3:25][NH:26][CH3:27]>COCCOC>[CH3:25][N:26]([CH3:27])[C:2]1[CH:7]=[C:6]([C:8]2[C:9]([C:20]3[O:21][CH:22]=[CH:23][CH:24]=3)=[N:10][C:11]([NH2:19])=[N:12][C:13]=2[C:14]2[O:15][CH:16]=[CH:17][CH:18]=2)[CH:5]=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 674DimethylamineHCID 23020419HCID 23020419、化合物

生成物 1

HCID 23020406HCID 23020406、化合物収率 43%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
70 °C

実験手順

In an autoclave, 5-(2-fluoro-4-pyridyl)-4,6-di(2-furyl)-2-pyrimidinamine (200 mg, 0.621 mmol) was suspended in 1,2-dimethoxyethane (10 ml) and then a 50% dimethylamine aqueous solution (5 ml) was added thereto, followed by stirring at 70° C. After 11 hours, the reaction mixture was extracted with ethyl acetate, and the extract was washed with water and brine, dried over anhydrous sodium sulfate and then the filtrate was concentrated. The resulting solid was suspended in ethanol, collected by filtration and washed with ethanol, to give the title compound (92 mg, 43%) as a pale yellow solid.

後処理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washthe extract was washed with water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationthe filtrate was concentrated
  5. filtrationcollected by filtration
  6. washwashed with ethanol

出典と根拠

ORDレコード
ord-dcd8f28f93e046ddb67b0eb25cc63601
出典データセット
uspto-grants-2008_07
特許番号
US07396836B2

反応ノート

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