2,4,6-Trimethylaniline → 1-(3-Nitrophenyl)-3-(mesityl)thiourea

HRID 2235483

반응식

HRID 2235483 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([N:10]=[C:11]=[S:12])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[C:13]1([CH3:22])[CH:18]=[C:17]([CH3:19])[CH:16]=[C:15]([CH3:20])[C:14]=1[NH2:21]>CO>[N+:1]([C:4]1[CH:5]=[C:6]([NH:10][C:11]([NH:21][C:14]2[C:15]([CH3:20])=[CH:16][C:17]([CH3:19])=[CH:18][C:13]=2[CH3:22])=[S:12])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 69132,4,6-TrimethylanilineHCID 19050Benzene, 1-isothiocyanato-3-nitro-

생성물 1

HCID 204104451-(3-Nitrophenyl)-3-(mesityl)thiourea

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 2.25 g (12.5 mmol) of 3-nitrophenylisothiocyanate and 1.4 mL (10 mmol) of mesityl amine in 10 mL of methanol was stirred at room temperature for 2 h. The resulting precipitate was collected by filtration and dried to give a quantitative yield of 1-(3-nitrophenyl)-3-(mesityl)thiourea. To 1.8 g (5.7 mmol) of the thiourea thus prepared slurried in 20 mL of CCl4 was added 0.35 mL (6.9 mmol) of bromine. The mixture was heated at reflux for 4 h, allowed to cool to room temperature and diluted with dichloromethane. This solution was washed successively with saturated sodium bicarbonate, water and brine before being dried over sodium sulfate. The solution was filtered, concentrated in vacuo and the resulting crude title compound was obtained in quantitative yield and was used without further purification.

후처리

  1. filtrationThe resulting precipitate was collected by filtration
  2. customdried

출처 및 근거

ORD 기록
ord-15eb015dcaf2471c83458d0635993b63
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07714009B2

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