creatinine → 1-(Tetrahydro-1-methyl-4-oxo-1H-imidazol-2-ylidene)-3-(2-thienyl) urea

HRID 904164

반응식

HRID 904164 반응식
[CH3:1][N:2]1[C:7]([NH2:8])=[N:6][C:4](=[O:5])[CH2:3]1.[S:9]1[CH:13]=[CH:12][CH:11]=[C:10]1[N:14]=[C:15]=[O:16]>CN(C=O)C.C1(C)C=CC=CC=1>[CH3:1][N:2]1[CH2:3][C:4](=[O:5])[NH:6][C:7]1=[N:8][C:15]([NH:14][C:10]1[S:9][CH:13]=[CH:12][CH:11]=1)=[O:16]

참가 물질

5

반응물 2

HCID 588creatinineHCID 27763752-Isocyanatothiophene

생성물 1

HCID 1359994131-(Tetrahydro-1-methyl-4-oxo-1H-imidazol-2-ylidene)-3-(2-thienyl) urea수율 30.3%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6228Dimethylformamide용매

반응 조건

온도
55 °C

실험 절차

To 9.4 g (83 mM) of creatinine in 100 ml of anhydrous DMF was added with stirring of solution of 9.2 g (75 mM) 2-thienyl isocyanate in 60 ml of toluene. After the addition was completed, the mixture was stirred at 55° C. for 1 hr., cooled, and the solvents removed in vacuo. The residue was recrystallized first from ethanol and then ethyl acetate (treated with charcoal) to give 5.3 g of the above urea as an off-white solid, m.p. 191°-192° C. (dec.).

후처리

  1. additionAfter the addition
  2. temperature, cooled
  3. customthe solvents removed in vacuo
  4. customThe residue was recrystallized first from ethanol

출처 및 근거

ORD 기록
ord-a723790e1f30406dbbcc7096558141ca
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04230713

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