4-Benzylpiperidine → HCID 69420844, 화합물

HRID 1357043노트

반응식

HRID 1357043 반응식
[CH3:1][O:2][C:3]1[C:4]([C:12]([OH:14])=O)=[CH:5][C:6]2[NH:10][CH:9]=[N:8][C:7]=2[CH:11]=1.CC[N:17]=C=NCCCN(C)C.Cl.[CH2:27]([CH:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>CN(C1C=CN=CC=1)C.CN(C=O)C.C(Cl)Cl>[CH3:1][O:2][C:3]1[C:4]([C:12]([NH2:17])=[O:14])=[CH:5][C:6]2[NH:10][C:9]([N:37]3[CH2:38][CH2:39][CH:34]([CH2:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[CH2:35][CH2:36]3)=[N:8][C:7]=2[CH:11]=1

참가 물질

6

반응물 3

HCID 317384-BenzylpiperidineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 185048955-Methoxy-1H-benzimidazole-6-carboxylic acid

생성물 1

HCID 69420844HCID 69420844, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 22350042dichloromethane N,N-dimethylformamide용매

실험 절차

6-methoxy-5-benzimidazole carboxylic acid, (1 equivalent) was treated with 1.1 equivalent of EDAC.HCl and 1 equivalent of 4-benzylpiperidine in the presence of a catalytic amount of DMAP in DMF/DCM 1:1 for 3-6 hrs. The reaction mixture was then concentrated and taken up in ethyl acetate. After washing with 5% aq. Sodium carbonate and a solution of saturated sodium chloride, the organic layer was dried over anhydrous sodium sulfate and concentrated to give crude material. This crude material was purified by chromatography on silica. M+ 349, Exp. 349.

후처리

  1. concentrationThe reaction mixture was then concentrated
  2. washAfter washing with 5% aq. Sodium carbonate
  3. dry with materiala solution of saturated sodium chloride, the organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customto give crude material
  6. customThis crude material was purified by chromatography on silica

출처 및 근거

ORD 기록
ord-e3a26c0ff6f34920b9bbea0de0aa0ed9
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06589954B1

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