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Sodium Hydroxide → (3-Bromo-5-pyrazol-1-yl-phenyl)-thiourea

HRID 447014
ノート
印刷プレビュー

反応式

HRID 447014 の反応式
[OH-].[Na+].C([NH:11][C:12]([NH:14][C:15]1[CH:20]=[C:19]([N:21]2[CH:25]=[CH:24][CH:23]=[N:22]2)[CH:18]=[C:17]([Br:26])[CH:16]=1)=[S:13])(=O)C1C=CC=CC=1>O.C1COCC1>[Br:26][C:17]1[CH:16]=[C:15]([NH:14][C:12]([NH2:11])=[S:13])[CH:20]=[C:19]([N:21]2[CH:25]=[CH:24][CH:23]=[N:22]2)[CH:18]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 57813664HCID 57813664、化合物

生成物 1

HCID 57813577(3-Bromo-5-pyrazol-1-yl-phenyl)-thiourea収率 85.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

A solution of NaOH (0.13 g, 3.35 mmol) dissolved in 1.0 mL of H2O was added to a solution of 1-Benzoyl-3-(3-bromo-5-pyrazol-1-yl-phenyl)-thiourea 3 (0.27 g, 0.67 mmol) in 5.0 mL of THF. The resulting reaction mixture was stirred at 70° C. for 12 hours. THF was distilled off and extracted with ethyl acetate (×3). The combined organic layer was dried over Na2SO4, filtered and distilled off to get the crude residue that was washed with 2% Ethyl acetate-hexane to obtain the desired compound (0.17 g, 85%).

後処理

  1. customThe resulting reaction mixture
  2. distillationTHF was distilled off
  3. extractionextracted with ethyl acetate (×3)
  4. dry with materialThe combined organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. distillationdistilled off
  7. customto get the crude residue that
  8. washwas washed with 2% Ethyl acetate-hexane

出典と根拠

ORDレコード
ord-1aaa361df4ff4b48b0fad846bc791a69
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08481544B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート