4-Benzylpiperidine → HCID 69420844、化合物

HRID 457764ノート

反応式

HRID 457764 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 69420844HCID 69420844、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 22350042dichloromethane N,N-dimethylformamide溶媒

実験手順

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 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.

後処理

  1. concentrationThe reaction mixture was then concentrated
  2. washAfter washing with 5% aq. Sodium carbonate a solution of saturated sodium chloride
  3. dry with materialthe 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

出典と根拠

ORDレコード
ord-e711e092f8594141b61b7aba4b70a11a
出典データセット
uspto-grants-2007_03
特許番号
US07189739B2

反応ノート

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