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

HRID 1427141
ノート
印刷プレビュー

反応式

HRID 1427141 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-a123dec21bf14a27916ce78c16a42179
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08933098B2

反応ノート

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