Sodium Hydroxide → HCID 58033225、化合物

HRID 447065ノート

反応式

HRID 447065 の反応式
C([NH:9][C:10]([NH:12][C:13]1[CH:18]=[C:17]([Br:19])[N:16]=[C:15]([Br:20])[CH:14]=1)=[S:11])(=O)C1C=CC=CC=1.[OH-].[Na+]>C1COCC1>[Br:20][C:15]1[CH:14]=[C:13]([NH:12][C:10]([NH2:9])=[S:11])[CH:18]=[C:17]([Br:19])[N:16]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 58033240HCID 58033240、化合物

生成物 1

HCID 58033225HCID 58033225、化合物収率 87.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
62.5 °C

実験手順

To a solution of 1-benzoyl-3-(2,6-dibromo-pyridin-4-yl)-thiourea (1.0 g, 2.14 mmol) in THF (50 mL) was added NaOH solution (0.48 in 20 mL H2O) at room temperature. The reaction mixture was heated up to 60-65° C. overnight. After completion of reaction (TLC monitoring) THF was distilled off followed by addition of water, and extraction with ethyl acetate (2×50 mL). The combined organic layers were dried over anhydrous Na2SO4, filtered and evaporated to dryness under reduced pressure. The crude residue was washed with mixture of ethyl acetate:hexane (30:70) and dried under high vacuum to get the desired product as a white solid (0.58 g, 78%).

後処理

  1. distillationwas distilled off
  2. additionfollowed by addition of water, and extraction with ethyl acetate (2×50 mL)
  3. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  4. filtrationfiltered
  5. customevaporated to dryness under reduced pressure
  6. washThe crude residue was washed with mixture of ethyl acetate:hexane (30:70)
  7. customdried under high vacuum

出典と根拠

ORDレコード
ord-147f7f3873a04c048314a561558492fe
出典データセット
uspto-grants-2013_07
特許番号
US08481544B2

反応ノート

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