Sodium → HCID 23020439、化合物

HRID 747166ノート

反応式

HRID 747166 の反応式
[Na].F[C:3]1[CH:8]=[C:7]([C:9]2[C:10]([C:21]3[O:22][CH:23]=[CH:24][CH:25]=3)=[N:11][C:12]([NH2:20])=[N:13][C:14]=2[C:15]2[O:16][CH:17]=[CH:18][CH:19]=2)[CH:6]=[CH:5][N:4]=1>C(O)CCC>[CH2:15]([O:16][C:3]1[CH:8]=[C:7]([C:9]2[C:10]([C:21]3[O:22][CH:23]=[CH:24][CH:25]=3)=[N:11][C:12]([NH2:20])=[N:13][C:14]=2[C:15]2[O:16][CH:17]=[CH:18][CH:19]=2)[CH:6]=[CH:5][N:4]=1)[CH2:14][CH2:9][CH3:7]

参加物

4

反応物 2

HCID 5360545SodiumHCID 23020419HCID 23020419、化合物

生成物 1

HCID 23020439HCID 23020439、化合物収率 108%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

In a reaction vessel, sodium (21 mg, 0.931 mmol) was dissolved in n-butanol (4 ml) and then 5-(2-fluoro-4-pyridyl)-4,6-di(2-furyl)-2-pyrimidinamine (100 mg, 0.310 mmol) was added thereto, followed by stirring under reflux for 5 hours under an atmosphere of nitrogen gas. The reaction was terminated by adding water thereto. Then, the reaction mixture was extracted with ethyl acetate, 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 (63 mg, 54%) as a pale yellow solid.

後処理

  1. temperatureunder reflux for 5 hours under an atmosphere of nitrogen gas
  2. customThe reaction was terminated
  3. additionby adding water
  4. extractionThen, the reaction mixture was extracted with ethyl acetate
  5. washwashed with water and brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationthe filtrate was concentrated
  8. filtrationcollected by filtration
  9. washwashed with ethanol

出典と根拠

ORDレコード
ord-e04d12db90154c5a916a472b01277a57
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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