Ammonium Acetate → N-(5-Phenyl-1,3,4-thiadiazol-2-yl)thiourea

HRID 1971462ノート

反応式

HRID 1971462 の反応式
[C:1]1([C:7]2[S:11][C:10]([NH:12][C:13]([N:15]3C=CN=C3)=[S:14])=[N:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])(=O)C.[NH4+]>C(O)C>[C:1]1([C:7]2[S:11][C:10]([NH:12][C:13]([NH2:15])=[S:14])=[N:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 86657910HCID 86657910、化合物

生成物 1

HCID 12388765N-(5-Phenyl-1,3,4-thiadiazol-2-yl)thiourea

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
90 °C

実験手順

1.0 g of the crude mixture with N-(5-phenyl-1,3,4-thiadiazole-2-yl)-1H-imidazole-1-carbothioamide was combined with 0.536 g (6.96 mmol) ammonium acetate in 4 ml ethanol. The reaction mixture was heated in the microwave (at 100 Watt) for 30 minutes at 90° C. After completion of the reaction, the solvent was distilled off under vacuum, and water was added to the residue formed. After extraction with CH2Cl2 and drying of the organic phase with magnesium sulfate, the product crystallized out of the organic solvent and, after filtration, was washed with diethylether. 0.52 g of the N-(5-phenyl-1,3,4-thiadiazole-2-yl)-thiourea was obtained.

後処理

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off under vacuum, and water
  3. additionwas added to the residue
  4. customformed
  5. extractionAfter extraction with CH2Cl2
  6. dry with materialdrying of the organic phase with magnesium sulfate
  7. customthe product crystallized out of the organic solvent
  8. filtrationafter filtration
  9. washwas washed with diethylether

出典と根拠

ORDレコード
ord-a31afdb748e44d0a90dc5fe8d2f1d142
出典データセット
uspto-grants-2013_04
特許番号
US08431604B2

反応ノート

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