Dimethylformamide → HCID 136334024, 화합물

HRID 2089626노트

반응식

HRID 2089626 반응식
C(O)(=O)C.[F:5][C:6]1[C:11]([O:12][CH2:13][CH2:14][OH:15])=[CH:10][C:9]([O:16][CH3:17])=[CH:8][C:7]=1[CH:18]([NH:31][C:32]1[CH:40]=[CH:39][C:35]([C:36]([NH2:38])=[NH:37])=[CH:34][CH:33]=1)[C:19]1[NH:23][C:22](=[O:24])[N:21]([C:25]2[N:30]=[CH:29][CH:28]=[CH:27][N:26]=2)[N:20]=1.CN(C=O)C.[N+](C1C=CC([O:55][C:56](=O)[O:57][CH2:58][C:59]([CH3:62])([CH3:61])[CH3:60])=CC=1)([O-])=O.C(N(CC)CC)C>C(O)(=O)C>[CH3:60][C:59]([CH3:62])([CH3:61])[CH2:58][O:57][C:56](=[O:55])[N:37]=[C:36]([NH2:38])[C:35]1[CH:34]=[CH:33][C:32]([NH:31][CH:18]([C:7]2[CH:8]=[C:9]([O:16][CH3:17])[CH:10]=[C:11]([O:12][CH2:13][CH2:14][OH:15])[C:6]=2[F:5])[C:19]2[NH:23][C:22](=[O:24])[N:21]([C:25]3[N:26]=[CH:27][CH:28]=[CH:29][N:30]=3)[N:20]=2)=[CH:40][CH:39]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 22389509Carbonic acid 2,2-dimethylpropyl ester 4-nitrophenyl esterHCID 1363340234-({[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl}amino)benzamidine acetic acid salt

생성물 1

HCID 136334024HCID 136334024, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a mixture of 4-({[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl}amino)benzamidine acetic acid salt (6 g) and DMF (500 mL), carbonic acid 2,2-dimethylpropyl ester 4-nitrophenyl ester [CAS No. 158810-98-1] (3.06 g) and triethylamine (4.64 mL) were added, and the resulting mixture was stirred overnight at room temperature. Acetic acid (5 mL) was added to the reaction solution, and the solvent was evaporated under reduced pressure. The residue obtained was purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate) to obtain the captioned compound (6.5 g).

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. customThe residue obtained
  3. customwas purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate)

출처 및 근거

ORD 기록
ord-eeee7642280c481f937ef8f4c8be72c3
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08436009B2

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