1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 10216398、化合物

HRID 988289ノート

反応式

HRID 988289 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][CH:9]([N:13]([CH:17]3[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)[CH2:14][CH2:15][CH3:16])[CH2:10]2)=[CH:5][CH:4]=1.[C:23]([N:26]1[CH2:31][CH2:30]C(C(O)=O)[CH2:28][CH2:27]1)(=[O:25])C.CCN=C=NCCCN(C)C.C1C=CC2N([OH:55])N=NC=2C=1>CCN(C(C)C)C(C)C>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][CH:9]([N:13]([CH2:14][CH2:15][CH3:16])[CH:17]3[CH2:18][CH2:19][N:20]([C:23]([N:26]4[CH2:27][CH2:28][O:55][CH2:30][CH2:31]4)=[O:25])[CH2:21][CH2:22]3)[CH2:10]2)=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 1172551-Acetylpiperidine-4-carboxylic acidHCID 12135182(7-Methoxy-1,2,3,4-tetrahydro-naphthalen-2-yl)-piperidin-4-yl-propyl-amine

生成物 1

HCID 10216398HCID 10216398、化合物

試薬・触媒・溶媒 1

HCID 81531Diisopropylethylamine溶媒

反応条件

温度
25 °C

実験手順

To a solution of (7-methoxy-1,2,3,4-tetrahydro-naphthalen-2-yl)-piperidin-4-yl-propyl-amine (200 μL of 0.25 M in dimethyl formamide, 50 μmole) was added 1-acetylpiperidine-4-carboxylic acid (220 μL of 0.25M in DMF), 300 μL of EDCI (0.25M in DMF) and 220 uL of HOBT (0.25M in DMF) and 30 μL DIEA. The solution was allowed to stir for 48 h at 25° C. under N2. Concentrated in vacuo. The final product was isolated by preparative RPHPLC (YMC Combiprep ODS-A column, 10-90% acetonitrile: water (0.1% TFA)) to afford 1-(4-{4-[(7-methoxy-1,2,3,4-tetrahydro-naphthalen-2-yl)-propyl-amino]-piperidine-1-carbonyl}-piperidin-1-yl)-ethanone 2 (5.2 mg ), [M+H]+=456.

後処理

  1. concentrationConcentrated in vacuo

出典と根拠

ORDレコード
ord-332abbc027d94324baedba80f0b58fcb
出典データセット
uspto-grants-2003_10
特許番号
US06635658B2

反応ノート

読み込み中…