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Trimethylamine → Methyl 3-[[5-bromo-2-(trifluoromethyl)benzoyl]amino]-2,4-dimethyl-benzoate

HRID 239990
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HRID 239990 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:11]([F:14])([F:13])[F:12])=[C:6]([CH:10]=1)[C:7]([OH:9])=O.N[C:16]1(C)[CH:25]=[C:24](C)[CH:23]=[C:18]([C:19]([O:21][CH3:22])=[O:20])[CH2:17]1.C[N:29]([CH3:31])C.[CH3:32]CCP1(OP(CCC)(=O)OP(CCC)(=O)O1)=O>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:11]([F:14])([F:13])[F:12])=[C:6]([CH:10]=1)[C:7]([NH:29][C:31]1[C:17]([CH3:32])=[C:18]([CH:23]=[CH:24][C:25]=1[CH3:16])[C:19]([O:21][CH3:22])=[O:20])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1146TrimethylamineHCID 111923Propylphosphonic anhydrideHCID 509981405-Bromo-2-trifluoromethylbenzoic acidHCID 86707353Methyl 3-amino-3,5-dimethylbenzoate

생성물 1

HCID 86707375Methyl 3-[[5-bromo-2-(trifluoromethyl)benzoyl]amino]-2,4-dimethyl-benzoate수율 56.5%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

To a solution of 5-bromo-2-(trifluoromethyl)benzoic acid (1.0 g, 3.53 mmol) in CH2Cl2 (6 ml) at room temperature are added methyl 3-amino-3,5-dimethylbenzoate (0.44 g, 2.47 mmol, see preparation 12) and trimethylamine (1.0 ml, 7.06 mmol). After stirring the reaction mixture for 10 minutes, 1-propanephosphonic acid cyclic anhydride (50% solution in ethyl acetate, 5.6 ml, 8.83 mmol) is added via syringe. After 14 hours at ambient temperature, the reaction mixture is diluted with CH2Cl2, washed with water and brine. The organic layers are combined and dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The resulting residue is purified by flash chromatography (silica gel) using 20% ethyl acetate in hexanes to give the title compound as a white solid (0.6 g, 39%).

후처리

  1. waitAfter 14 hours at ambient temperature
  2. washwashed with water and brine
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue is purified by flash chromatography (silica gel)

출처 및 근거

ORD 기록
ord-f428251c514c41e1818ff8999a0b1fdb
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08642768B2

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