Potassium Carbonate → HCID 6992124、化合物

HRID 1899395ノート

反応式

HRID 1899395 の反応式
Br[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([F:12])=[CH:8][C:7]=1[F:13])=[O:4].[O:14]=[C:15]1[N:19]([CH:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)[C:18]2[CH:26]=[CH:27][CH:28]=[CH:29][C:17]=2[NH:16]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:13][C:7]1[CH:8]=[C:9]([F:12])[CH:10]=[CH:11][C:6]=1[NH:5][C:3](=[O:4])[CH2:2][N:23]1[CH2:22][CH2:21][CH:20]([N:19]2[C:18]3[CH:26]=[CH:27][CH:28]=[CH:29][C:17]=3[NH:16][C:15]2=[O:14])[CH2:25][CH2:24]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 886381,3-Dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-oneHCID 34164012-bromo-N-(2,4-difluorophenyl)acetamide

生成物 1

HCID 6992124HCID 6992124、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4 g (16 mmol) of the bromoacetanilide from Example I and 4.2 g (19 mmol) of 4-(2-oxo-1-benzimidazolinyl)piperidine in 50 ml of dimethylformamide are stirred at RT for 18 h with 2.6 g (19 mmol) of potassium carbonate. The solid is then filtered off with suction, the filtrate is partitioned between ethyl acetate and water, and the aqueous phase is extracted 3 times with ethyl acetate. The organic phases are combined, washed with saturated sodium chloride solution, dried (MgSO4) and concentrated. The residue obtained is triturated with ether, and the solid is filtered off and then recrystallized from methanol.

後処理

  1. filtrationThe solid is then filtered off with suction
  2. customthe filtrate is partitioned between ethyl acetate and water
  3. extractionthe aqueous phase is extracted 3 times with ethyl acetate
  4. washwashed with saturated sodium chloride solution
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customThe residue obtained
  8. customis triturated with ether
  9. filtrationthe solid is filtered off
  10. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-2875453875f84c3795d8e3f1ab29af6e
出典データセット
uspto-grants-1996_11
特許番号
US05571921

反応ノート

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