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

HRID 447936노트

반응식

HRID 447936 반응식
[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

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 86657910HCID 86657910, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-173a8d8b0c434eaea343b8f079821236
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481576B2

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