Water → 1-Benzoyl-3-(3-bromo-5-iodophenyl)-thiourea

HRID 446997

反応式

HRID 446997 の反応式
[S-:1][C:2]#[N:3].[NH4+].[C:5](Cl)(=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Br:14][C:15]1[CH:16]=[C:17]([CH:19]=[C:20]([I:22])[CH:21]=1)[NH2:18].O>CC(C)=O>[C:5]([NH:3][C:2]([NH:18][C:17]1[CH:19]=[C:20]([I:22])[CH:21]=[C:15]([Br:14])[CH:16]=1)=[S:1])(=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 7412Benzoyl chlorideHCID 15666Ammonium thiocyanateHCID 454803883-Bromo-5-iodoaniline

生成物 1

HCID 578136521-Benzoyl-3-(3-bromo-5-iodophenyl)-thiourea収率 84.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

A solution of ammonium thiocyanate (4.45 g, 0.0585 mol) in anhydrous acetone (48 ml) was treated dropwise with benzoyl chloride (6.47 ml, 0.05583 mol) and stirred at ambient temperature for 1 h. A solution of 3-Bromo-5-iodoaniline (15.85 g, 0.05319 mol) in anhydrous acetone (48 ml) was then added in one portion and the mixture stirred at ambient temperature for 16 h. The resultant suspension was poured into water (300 ml) and stirred for 0.5 h. The precipitated solid was collected by filtration washed with water followed by 40-60° petroleum ether and dried in vacuo to afford 1-Benzoyl-3-(3-bromo-5-iodo-phenyl)-thiourea (20.70 g, 84%).

後処理

  1. stirringthe mixture stirred at ambient temperature for 16 h
  2. stirringstirred for 0.5 h
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water
  5. customfollowed by 40-60°
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-e4e4a2ffc5494a068330c97663dcfce6
出典データセット
uspto-grants-2013_07
特許番号
US08481544B2

関連ノート

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