Diisopropylethylamine → N-(3-amino-4-thienyl)-N'-(4-methyl-3-thienyl)thiourea

HRID 349412

반응식

HRID 349412 반응식
Cl.Cl.[NH2:3][C:4]1[C:8]([NH2:9])=[CH:7][S:6][CH:5]=1.C(N(C(C)C)C(C)C)C.[CH3:19][C:20]1[C:21]([N:25]=[C:26]=[S:27])=[CH:22][S:23][CH:24]=1>O1CCCC1>[NH2:3][C:4]1[C:8]([NH:9][C:26]([NH:25][C:21]2[C:20]([CH3:19])=[CH:24][S:23][CH:22]=2)=[S:27])=[CH:7][S:6][CH:5]=1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 127073423,4-Diaminothiophene dihydrochlorideHCID 221398273-Isothiocyanato-4-methylthiophene

생성물 1

HCID 86037734N-(3-amino-4-thienyl)-N'-(4-methyl-3-thienyl)thiourea

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 1.87 g of 3,4-diaminothiophene dihydrochloride, 60 ml of anhydrous tetrahydrofuran (THF) and 2.58 g of N-ethyl-N,N-diisopropylamine was stirred at room temperature for 30 minutes and then admixed with 1.5 g of 4-methyl-3-thienyl isothiocyanate. After stirring over approx. 18 hours, the solvent was distilled off, 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 once again distilled off. The N-(3-amino-4-thienyl)-N′-(4-methyl-3-thienyl)thiourea was obtained as an amorphous foamy solid.

후처리

  1. stirringAfter stirring over approx. 18 hours
  2. distillationthe solvent was distilled off
  3. extractionthe residue admixed with water and extracted repeatedly with ethyl acetate
  4. additionAfter the combined organic phases had been treated with activated carbon, they
  5. dry with materialwere dried over sodium sulfate
  6. distillationthe solvent was once again distilled off

출처 및 근거

ORD 기록
ord-b42dad8b0c4d4bada62dd01825bed579
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179830B2

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