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Potassium Hydroxide → HCID 25190386、化合物

HRID 219765
ノート
印刷プレビュー

反応式

HRID 219765 の反応式
[F:1][C:2]([F:35])([F:34])[C:3]1[CH:11]=[C:10]([C:12]#[N:13])[CH:9]=[C:8]2[C:4]=1[C:5]([NH:22][C:23](=[O:33])[CH2:24][N:25]1[CH2:30][CH2:29][N:28]([CH2:31][CH3:32])[CH2:27][CH2:26]1)([C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=1)[C:6](=[O:14])[NH:7]2.[OH-:36].[K+]>CC(O)(C)C>[Cl:21][C:18]1[CH:17]=[CH:16][C:15]([C:5]2([NH:22][C:23](=[O:33])[CH2:24][N:25]3[CH2:26][CH2:27][N:28]([CH2:31][CH3:32])[CH2:29][CH2:30]3)[C:4]3[C:8](=[CH:9][C:10]([C:12]([NH2:13])=[O:36])=[CH:11][C:3]=3[C:2]([F:1])([F:34])[F:35])[NH:7][C:6]2=[O:14])=[CH:20][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 66602253HCID 66602253、化合物

生成物 1

HCID 25190386HCID 25190386、化合物収率 60.4%

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

0.16 g of the product obtained in Example 4, 0.47 g of potassium hydroxide and 7 ml of t-BuOH are placed in a round-bottomed flask equipped with a magnetic stirrer. The mixture is left to react at 50° C. for 5 hours. The resulting mixture is filtered through Celite and washed with THF. The filtrate is evaporated under vacuum and the residue is taken up in ethyl acetate and washed with water. The organic phase is dried over Na2SO4, filtered and evaporated under vacuum. 100 mg of an oil are obtained, which oil is purified by flash chromatography, eluting with 8/2 ethyl acetate/methanol. 10 mg of white solid are isolated.

後処理

  1. customequipped with a magnetic stirrer
  2. waitThe mixture is left
  3. customto react at 50° C. for 5 hours
  4. filtrationThe resulting mixture is filtered through Celite
  5. washwashed with THF
  6. customThe filtrate is evaporated under vacuum
  7. washwashed with water
  8. dry with materialThe organic phase is dried over Na2SO4
  9. filtrationfiltered
  10. customevaporated under vacuum

出典と根拠

ORDレコード
ord-a5f34ff25a584c5ba21faf4efbd1e5d1
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08202871B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート