Triethylamine → HCID 178522952, 화합물

HRID 1071998노트

반응식

HRID 1071998 반응식
Cl.Cl.[NH:3]1[C:11]2[CH2:10][CH2:9][NH:8][CH2:7][C:6]=2[N:5]=[CH:4]1.C(N(CC)CC)C.[Cl:19][C:20]1[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:21]=1[CH2:22][N:23]=[C:24]=[O:25]>C(O)C>[Cl:19][C:20]1[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:21]=1[CH2:22][NH:23][C:24]([N:8]1[CH2:9][CH2:10][C:11]2[NH:3][CH:4]=[N:5][C:6]=2[CH2:7]1)=[O:25]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 46127082,4-Dichlorobenzyl isocyanateHCID 164180044,5,6,7-Tetrahydro-3H-imidazo[4,5-c]pyridine--hydrogen chloride (1/2)

생성물 1

HCID 178522952HCID 178522952, 화합물수율 37%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a mixture of 4,5,6,7-tetrahydroimidazo[4,5-c]pyridine dihydrochloride (0.50 g, 2.55 mmol), ethanol (10 mL) and triethylamine (1.10 mL, 7.89 mmol), 2,4-dichlorobenzyl isocyanate (0.52 g, 2.57 mmol) was added. The resulting mixture was stirred at room temperature for 16 h and then concentrated under reduced pressure. The residue was distributed between water (20 mL) and ethyl acetate (75 mL). The organic phase was washed with water (10 mL) and brine (10 mL), dried (MgSO4) and concentrated under reduced pressure. The residue was triturated in diethylether (50 mL) and the crude product was filtered off. Recrystallization from acetone (25 mL) gave 0.30 g (37%) of the title urea as a colourless solid.

후처리

  1. additionwas added
  2. concentrationconcentrated under reduced pressure
  3. washThe organic phase was washed with water (10 mL) and brine (10 mL)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was triturated in diethylether (50 mL)
  7. filtrationthe crude product was filtered off
  8. customRecrystallization from acetone (25 mL)

출처 및 근거

ORD 기록
ord-05512a3be2834b409d2d52b1282b104e
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06908926B1

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