Benzoyl chloride → Thiourea, [3-(dimethylamino)-2-methylphenyl]-

HRID 24981ノート

反応式

HRID 24981 の反応式
[CH3:1][N:2]([CH3:11])[C:3]1[C:4]([CH3:10])=[C:5]([CH:7]=[CH:8][CH:9]=1)[NH2:6].[C:12]([S-:14])#[N:13].[K+].C(Cl)(=O)C1C=CC=CC=1.[OH-].[K+]>C(O)C.O.CC(C)=O>[CH3:1][N:2]([CH3:11])[C:3]1[C:4]([CH3:10])=[C:5]([NH:6][C:12]([NH2:13])=[S:14])[CH:7]=[CH:8][CH:9]=1

参加物

8

反応物 4

HCID 7412Benzoyl chlorideHCID 14797Potassium HydroxideHCID 516872Potassium thiocyanateHCID 111373411-N,1-N,2-trimethylbenzene-1,3-diamine

生成物 1

HCID 10856728Thiourea, [3-(dimethylamino)-2-methylphenyl]-収率 91.3%

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 702Ethanol溶媒2 回HCID 962Water溶媒2 回

実験手順

57 g of 3-dimethylamino-2-methyl-aniline, 1.15 liters of acetone, 36.6 g of KSCN and 43.8 ml of benzoylchloride are refluxed together for 3 hours. After cooling to ambient temperature the reaction mixture is poured onto 2.4 kg of crushed ice. The precipitate obtained is heated to 60° C. for 2 hours together with 85 g of KOH, 85 ml of water and 255 ml of ethanol. After the addition of 850 ml of water the ethanol is distilled off under reduced pressure. After the resulting precipitate has been worked up, 72 g of N-(3-dimethylamino-2-methylphenyl)-thiourea are obtained.

後処理

  1. customThe precipitate obtained
  2. distillationis distilled off under reduced pressure

出典と根拠

ORDレコード
ord-4af9c31168e94a3c9a00a55a1e5628d3
出典データセット
uspto-grants-2005_02
特許番号
US06858594B2

反応ノート

読み込み中…