Potassium Carbonate → HCID 6992124, 화합물

HRID 1899395노트

반응식

HRID 1899395 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 6992124HCID 6992124, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2875453875f84c3795d8e3f1ab29af6e
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05571921

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