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

HRID 1387390노트

반응식

HRID 1387390 반응식
[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

참가 물질

8

반응물 4

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

생성물 1

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

시약·촉매·용매 3

HCID 180Acetone용매HCID 702Ethanol용매2회HCID 962Water용매2회

실험 절차

57 g of 3-dimethylamino-2-methyl-aniline, 1.15 litres 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.

후처리

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

출처 및 근거

ORD 기록
ord-f9b0979c526b442197a4439f9870e3e6
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06268389B1

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