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1,1'-Carbonyldiimidazole → N-(1-(5-carbamoylpyridin-2-yl)piperidin-4-yl)-4-isopropylpiperazine-1-carboxamide

HRID 1504599
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HRID 1504599 반응식
Cl.[NH2:2][CH:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:17]=[CH:16][C:12]([C:13]([NH2:15])=[O:14])=[CH:11][N:10]=2)[CH2:5][CH2:4]1.[CH3:18][CH2:19][N:20]([CH:24]([CH3:26])[CH3:25])[CH:21](C)[CH3:22].[C:27](N1C=CN=C1)([N:29]1C=CN=C1)=[O:28].C(N1CCNCC1)(C)C>CN(C=O)C>[C:13]([C:12]1[CH:16]=[CH:17][C:9]([N:6]2[CH2:5][CH2:4][CH:3]([NH:2][C:27]([N:29]3[CH2:22][CH2:21][N:20]([CH:24]([CH3:26])[CH3:25])[CH2:19][CH2:18]3)=[O:28])[CH2:8][CH2:7]2)=[N:10][CH:11]=1)(=[O:14])[NH2:15]
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참가 물질

6

반응물 4

HCID 682631,1'-CarbonyldiimidazoleHCID 780131-IsopropylpiperazineHCID 81531DiisopropylethylamineHCID 693590386-(4-Aminopiperidin-1-yl)nicotinamide hydrochloride

생성물 1

HCID 86730057N-(1-(5-carbamoylpyridin-2-yl)piperidin-4-yl)-4-isopropylpiperazine-1-carboxamide수율 8%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

To a cooled solution (0-5° C.) of 6-(4-aminopiperidin-1-yl)nicotinamide hydrochloride (293 mg, 1 mmol) in 5 ml DMF was added DIPEA (645 mg, 2.2 mmol) and 1,1′-carbonyldiimidazole (170 mg, 1.05 mmol). After stirring for 1 h, 1-isopropylpiperazine (154 mg, 1.2 mmol) was added and the resulting mixture was warmed to room temperature for 16 h. The crude mixture was filtered through Celite and the filtrate was purified by preparative HPLC to give title compound (30 mg, 8%) as an off-white solid. [1HNMR (400 MHz, DMSO-d6) δ 8.60 (d, 1H), 7.94 (m, 1H), 7.73 (s, 1H), 7.10 (s, 1H), 6.86 (d, 1H), 6.21 (d, 1H), 4.37 (d, 2H), 3.65 (m, 1H), 3.23 (t, 4H), 2.94 (t, 2H) 2.62 (m, 1H), 2.34 (t, 4H), 1.78 (d, 2H), 1.36 (m, 2H), 0.96 (d, 6H); LCMS RtB=1.53 min, [M+H]+=375.2].

후처리

  1. filtrationThe crude mixture was filtered through Celite
  2. customthe filtrate was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-d6668632bbc64f18b9250b2827ba5cc7
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216182B2

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