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Diisopropylethylamine → 4'-Methyl-N-((6-methylpyridin-3-yl)methyl)-5-(methylsulfonyl)biphenyl-3-carboxamide

HRID 1845193
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HRID 1845193 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[C:12]([S:14]([CH3:17])(=[O:16])=[O:15])[CH:11]=[C:10]([C:18]([OH:20])=O)[CH:9]=2)=[CH:4][CH:3]=1.Cl.CN(C)CCCN=C=NCC.O.ON1C2C=CC=CC=2N=N1.[CH3:44][C:45]1[N:50]=[CH:49][C:48]([CH2:51][NH2:52])=[CH:47][CH:46]=1.C(N(CC)C(C)C)(C)C>C(Cl)Cl>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[C:12]([S:14]([CH3:17])(=[O:15])=[O:16])[CH:11]=[C:10]([C:18]([NH:52][CH2:51][C:48]3[CH:49]=[N:50][C:45]([CH3:44])=[CH:46][CH:47]=3)=[O:20])[CH:9]=2)=[CH:6][CH:7]=1
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참가 물질

7

반응물 5

HCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 12214337(6-Methylpyridin-3-yl)methanamineHCID 581879934'-Methyl-5-(methylsulfonyl)biphenyl-3-carboxylic acid

생성물 1

HCID 44223084
4'-Methyl-N-((6-methylpyridin-3-yl)methyl)-5-(methylsulfonyl)biphenyl-3-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a mixture of 4′-methyl-5-(methylsulfonyl)biphenyl-3-carboxylic acid (40 mg, 0.14 mmol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (53 mg, 0.28 mmol), 1-hydroxybenzotriazole hydrate (21 mg, 0.14 mmol), and CH2Cl2 (3 mL) were added (6-methylpyridin-3-yl)methanamine (25 mg, 0.21 mmol), and N,N-diisopropylethylamine (48 μL, 0.28 mmol). The mixture was stirred at room temperature overnight and then concentrated. The residue was purified by preparative HPLC (100×20.2 mm, C18 column; 30-80% CH3CN-water[10 mM Et2NH]) to afford a white solid.

후처리

  1. concentrationconcentrated
  2. customThe residue was purified by preparative HPLC (100×20.2 mm, C18 column; 30-80% CH3CN-water[10 mM Et2NH])
  3. customto afford a white solid

출처 및 근거

ORD 기록
ord-c170afbc6f2b4ca5abc439f359ea46ca
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946439B2

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