Urea → 1-Benzoyl-3-methyl-5-(3-trichloromethyl-1,2,4-thiadiazol-5-yl)biuret

HRID 27997

反応式

HRID 27997 の反応式
[CH3:1][NH:2][C:3]([NH:5][C:6]1[S:10][N:9]=[C:8]([C:11]([Cl:14])([Cl:13])[Cl:12])[N:7]=1)=[O:4].[C:15]([N:23]=[C:24]=[O:25])(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.NC(N)=O>C1C=CC=CC=1>[C:15]([NH:23][C:24]([N:2]([CH3:1])[C:3]([NH:5][C:6]1[S:10][N:9]=[C:8]([C:11]([Cl:12])([Cl:14])[Cl:13])[N:7]=1)=[O:4])=[O:25])(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

5

反応物 3

HCID 1176UreaHCID 78210Benzoyl isocyanateHCID 233412461-Methyl-3-(3-trichloromethyl-1,2,4-thiadiazol-5-yl)urea

生成物 1

HCID 233412431-Benzoyl-3-methyl-5-(3-trichloromethyl-1,2,4-thiadiazol-5-yl)biuret収率 35.5%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
145 °C

実験手順

A glass pressure vessel was charged with 5.5 grams (0.02 mole) 1-methyl-3-(3-trichloromethyl-1,2,4-thiadiazol-5-yl)urea, 3.2 grams (0.02 mole) benzoyl isocyanate and 50 milliliters benzene. A magnetic stirring bar was added and the vessel sealed. The stirred reaction mixture was heated at 145° C. for 1.5 hours and then allowed to cool to room temperature where 4.5 grams of starting urea precipitates. The urea was removed by filtration and the filtrate concentrated in vacuo to leave 3.0 grams of residue. Extraction of the residue with hot cyclohexane, followed by cooling the extract yielded 0.2 grams (11% selectivity) of pure product; m.p. 70° C.

後処理

  1. additionA magnetic stirring bar was added
  2. customthe vessel sealed
  3. customThe stirred reaction mixture
  4. customprecipitates
  5. customThe urea was removed by filtration
  6. concentrationthe filtrate concentrated in vacuo

出典と根拠

ORDレコード
ord-8612e1f7ac334909a950534ef2d2bb70
出典データセット
uspto-grants-1980_09
特許番号
US04224449

関連ノート

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