Tetrahydrofuran → N-(3-Amino-4-thienyl)-N'-(2,6-dichlorophenyl)thiourea

HRID 349413

반응식

HRID 349413 반응식
Cl.Cl.[NH2:3][C:4]1[C:8]([NH2:9])=[CH:7][S:6][CH:5]=1.C1COCC1.C(N(C(C)C)C(C)C)C.[Cl:24][C:25]1[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[C:26]=1[N:32]=[C:33]=[S:34]>C(OCC)(=O)C>[NH2:3][C:4]1[C:8]([NH:9][C:33]([NH:32][C:26]2[C:27]([Cl:31])=[CH:28][CH:29]=[CH:30][C:25]=2[Cl:24])=[S:34])=[CH:7][S:6][CH:5]=1

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 81531DiisopropylethylamineHCID 1232391,3-Dichloro-2-isothiocyanatobenzeneHCID 127073423,4-Diaminothiophene dihydrochloride

생성물 1

HCID 86037735N-(3-Amino-4-thienyl)-N'-(2,6-dichlorophenyl)thiourea

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 1.87 g of 3,4-diaminothiophene dihydrochloride, 60 ml of anhydrous THF and 2.58 g of N-ethyl-N,N-diisopropylamine was stirred at room temperature for 30 minutes and then admixed with 2.04 g of 2,6-dichlorophenyl isothiocyanate. After the mixture had been heated to 40° C. for 10 minutes, it was stirred at room temperature for approx. 18 hours, and the solvent was distilled off, and the residue admixed with water and extracted repeatedly with ethyl acetate. After the combined organic phases had been treated with activated carbon, they were dried over sodium sulfate and the solvent was again distilled off. A crystalline solid was obtained and, after stirring with a little ethyl acetate, was filtered off. M.p. 165° C.

후처리

  1. temperatureAfter the mixture had been heated to 40° C. for 10 minutes
  2. stirringit was stirred at room temperature for approx. 18 hours
  3. distillationthe solvent was distilled off
  4. extractionthe residue admixed with water and extracted repeatedly with ethyl acetate
  5. additionAfter the combined organic phases had been treated with activated carbon, they
  6. dry with materialwere dried over sodium sulfate
  7. distillationthe solvent was again distilled off
  8. customA crystalline solid was obtained
  9. filtrationwas filtered off

출처 및 근거

ORD 기록
ord-241168cd9bac4a46b0fa26436f3bd4f8
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179830B2

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