Triethylamine → HCID 178522952、化合物

HRID 1071998ノート

反応式

HRID 1071998 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 178522952HCID 178522952、化合物収率 37%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-05512a3be2834b409d2d52b1282b104e
出典データセット
uspto-grants-2005_06
特許番号
US06908926B1

反応ノート

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