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1-Hydroxybenzotriazole → Biphenyl-4-carboxylicacid {2-[4-(2-chloro-pyridine-3-carbonyl)-piperazin-1-yl]-2-oxo-ethyl}-amide

HRID 1178096
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HRID 1178096 반응식
CCN(C(C)C)C(C)C.[Cl:10][C:11]1[N:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([OH:15])=O.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.[O:42]=[C:43]([N:60]1[CH2:65][CH2:64][NH:63][CH2:62][CH2:61]1)[CH2:44][NH:45][C:46]([C:48]1[CH:53]=[CH:52][C:51]([C:54]2[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=2)=[CH:50][CH:49]=1)=[O:47]>CN(C=O)C.O>[Cl:10][C:11]1[C:12]([C:13]([N:63]2[CH2:62][CH2:61][N:60]([C:43](=[O:42])[CH2:44][NH:45][C:46]([C:48]3[CH:53]=[CH:52][C:51]([C:54]4[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=4)=[CH:50][CH:49]=3)=[O:47])[CH2:65][CH2:64]2)=[O:15])=[CH:16][CH:17]=[CH:18][N:19]=1
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참가 물질

8

반응물 5

HCID 757711-HydroxybenzotriazoleHCID 762582-Chloronicotinic acidHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 57855677Biphenyl-4-carboxylicacid (2-oxo-2-piperazin-1-yl-ethyl)-amide

생성물 1

HCID 59559610
Biphenyl-4-carboxylicacid {2-[4-(2-chloro-pyridine-3-carbonyl)-piperazin-1-yl]-2-oxo-ethyl}-amide
수율 32.8%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

DIPEA (149.8 mg, 1.15 mmol) was added to a stirred solution of 2-chloro-nicotinic acid (40.5 mg, 0.26 mmol) in DMF (3 mL), HOBt (38.2 mg, 0.28 mmol) and EDCI.HCl (123.4 mg, 0.64 mmol) at room temperature. After 2 minutes biphenyl-4-carboxylicacid (2-oxo-2-piperazin-1-yl-ethyl)-amide (100 mg, 0.31 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added, and the resulting precipitate was filtered. The residue was purified by column chromatography (using 60-120 mesh silica gel and 90% EtOAc in hexane as eluent) to afford 39 mg (32.8% yield) of biphenyl-4-carboxylicacid {2-[4-(2-chloro-pyridine-3-carbonyl)-piperazin-1-yl]-2-oxo-ethyl}-amide, LC-MS purity: 89.81%, 1H NMR: (DMSO) δ 8.74-8.62 (bs, 1H), 8.56-8.46 (bs, 1H), 8.06-7.92 (d, 3H), 7.84-7.7 (q, 4H), 7.6-7.38 (m, 4H), 4.28-4.12 (d, 2H), 3.78-3.46 (bt, 6H), 3.28-3.18 (bs, 2H).

후처리

  1. filtrationthe resulting precipitate was filtered
  2. customThe residue was purified by column chromatography (using 60-120 mesh silica gel and 90% EtOAc in hexane as eluent)

출처 및 근거

ORD 기록
ord-a1631367b2b3478984adf3098881a9ff
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07842696B2

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