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Water → N-(2-Amino-5-methoxy-phenyl)-5-bromo-2-fluoro-benzamide

HRID 77077
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HRID 77077 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:11])=[C:6]([CH:10]=1)[C:7]([OH:9])=O.Cl.Cl.[CH3:14][O:15][C:16]1[CH:17]=[C:18]([NH2:23])[C:19]([NH2:22])=[CH:20][CH:21]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.O>ClCCl.CN(C=O)C>[NH2:22][C:19]1[CH:20]=[CH:21][C:16]([O:15][CH3:14])=[CH:17][C:18]=1[NH:23][C:7](=[O:9])[C:6]1[CH:10]=[C:2]([Br:1])[CH:3]=[CH:4][C:5]=1[F:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 27363155-Bromo-2-fluorobenzoic acidHCID 30851614-Methoxybenzene-1,2-diamine dihydrochlorideHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

생성물 1

HCID 63257662N-(2-Amino-5-methoxy-phenyl)-5-bromo-2-fluoro-benzamide수율 62.4%

시약·촉매·용매

2
HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

Method 6—Step a A mixture of 5-Bromo-2-fluoro-benzoic acid (1.50 g, 6.85 mmol), 4-methoxy-benzene-1,2-diamine dihydrochloride (1.77 g, 8.49 mmol), HATU (2.73 g, 7.19 mmol) and TEA (2.88 mL, 20.76 mmol) in dichloromethane (20 mL) and DMF (5 mL) was stirred at room temperature overnight, then water was added (50 mL), mixture was stirred for 2 h and left standing at room temperature overnight. The precipitate obtained was filtered off and dried to afford 1.45 g of the title compound (50%).

후처리

  1. stirringwas stirred for 2 h
  2. waitleft
  3. waitstanding at room temperature overnight
  4. customThe precipitate obtained
  5. filtrationwas filtered off
  6. customdried

출처 및 근거

ORD 기록
ord-d73d945322a94c8a9a3b8a50b768d317
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08835648B2

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