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Nicotinic Acid → N-[3-(4-Cyclohexylcarbamoyl-piperidin-1-ylmethyl)-phenyl]-nicotinamide

HRID 1486717
ノート
印刷プレビュー

反応式

HRID 1486717 の反応式
[CH:1]1([NH:7][C:8]([CH:10]2[CH2:15][CH2:14][N:13]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([NH2:23])[CH:18]=3)[CH2:12][CH2:11]2)=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:24](O)(=[O:31])[C:25]1[CH:30]=[CH:29][CH:28]=[N:27][CH:26]=1.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C.CCN=C=NCCCN(C)C.Cl>C(Cl)Cl.CN(C1C=CN=CC=1)C>[CH:1]1([NH:7][C:8]([CH:10]2[CH2:11][CH2:12][N:13]([CH2:16][C:17]3[CH:18]=[C:19]([NH:23][C:24](=[O:31])[C:25]4[CH:30]=[CH:29][CH:28]=[N:27][CH:26]=4)[CH:20]=[CH:21][CH:22]=3)[CH2:14][CH2:15]2)=[O:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 938Nicotinic AcidHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 867065241-(3-Amino-benzyl)-piperidine-4-carboxylic acid cyclohexylamide

生成物 1

HCID 129625936
N-[3-(4-Cyclohexylcarbamoyl-piperidin-1-ylmethyl)-phenyl]-nicotinamide

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒3 回

実験手順

To a solution of 1-(3-amino-benzyl)-piperidine-4-carboxylic acid cyclohexylamide BB-1 (200 mg, 0.57 mmol) in DCM (5 mL) are added successively nicotinic acid (70 mg, 0.57 mmol), HOBT (154 mg, 1.14 mmol), DMAP (14 mg, 0.11 mmol) and DIPEA (0.29 mL, 1.7 mmol). A solution of EDC hydrochloride (163 mg, 0.85 mmol) in DCM (2 mL) is added and the reaction mixture is stirred for 4 days at RT. The mixture is diluted with DCM (10 mL) and washed twice with sat.aq. NaHCO3 (20 mL). The combined organic phases are dried over MgSO4 and filtered. The solvent is evaporated under reduced pressure. The residue is dissolved in acetonitrile and purified by prep. HPLC E. LCMS C: tR=0.56 min; [M+H]+=421.4. 1H-NMR (DMSO-d6): δ 1.1-1.3 (m, 5H), 1.5-1.7 (m, 9H), 1.8-1.9 (m, 2H), 2.0-2.1 (m, 1H), 2.84 (d, J=9, 2H), 3.4-3.5 (m, 3H), 7.03 (d, J=7, 1H), 7.30 (t, J=7, 1H), 7.5-7.8 (m, 4H), 8.29 (d, J=8, 1H), 8.7-8.8 (m, 1H), 9.11 (s, 1H), 10.4 (s, 1H).

後処理

  1. washwashed twice with sat.aq
  2. dry with materialThe combined organic phases are dried over MgSO4
  3. filtrationfiltered
  4. customThe solvent is evaporated under reduced pressure
  5. dissolutionThe residue is dissolved in acetonitrile
  6. custompurified by prep

出典と根拠

ORDレコード
ord-1edd147d5dd54c99b0b28283cbb29adc
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428456B2

反応ノート

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