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Dimethylformamide → 4-(4-Trifluoromethylpyrid-3-ylcarbonylamino)-2-phenylbenzoic acid 2-trimethylsilylethyl ester

HRID 383129
ノート
印刷プレビュー

反応式

HRID 383129 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[C:8]([C:9]([OH:11])=O)=[CH:7][N:6]=[CH:5][CH:4]=1.[CH3:14][Si:15]([CH3:43])([CH3:42])[CH2:16][CH2:17][O:18][C:19](=[O:41])[C@H:20](CCSC)NC(=O)C1C=CC(N)=CC=1C1C=CC=CC=1.ON1[C:50](=O)[C:49]2[CH:52]=[CH:53][CH:54]=[CH:55][C:48]=2N=N1.CN(C)[CH2:58][CH2:59][CH2:60][N:61]=C=NCC.[CH3:67]N(C=O)C>C(OCC)(=O)C>[CH3:43][Si:15]([CH3:14])([CH3:42])[CH2:16][CH2:17][O:18][C:19](=[O:41])[C:20]1[CH:58]=[CH:59][C:60]([NH:61][C:9]([C:8]2[CH:7]=[N:6][CH:5]=[CH:4][C:3]=2[C:2]([F:1])([F:13])[F:12])=[O:11])=[CH:67][C:50]=1[C:49]1[CH:52]=[CH:53][CH:54]=[CH:55][CH:48]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 6228DimethylformamideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 730263-hydroxy-1,2,3-benzotriazin-4(3H)-oneHCID 27775493-Pyridinecarboxylic acid, 4-(trifluoromethyl)-HCID 67550574(4-Amino-2-phenylbenzoyl)methionine 2-trimethylsilylethyl ester

生成物 1

HCID 67550687
4-(4-Trifluoromethylpyrid-3-ylcarbonylamino)-2-phenylbenzoic acid 2-trimethylsilylethyl ester
収率 87%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 4-trifluoromethylnicotinic acid (472 mg, 2.46 mmol), the product of Example 283B (771 mg, 2.46 mmol), 3-hydroxy1,2,3-benzotriazin-4(3H)-one (481 mg, 2.95 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (566 mg, 2.95 mmol) in DMF (8 mL) was stirred room temperature for 15 hours. The reaction mixture was diluted with ethyl acetate (100 mL), washed with water and brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography (30% ethyl acetate-hexane) to give the title compound (1.04 g, 87%).

後処理

  1. washwashed with water and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography (30% ethyl acetate-hexane)

出典と根拠

ORDレコード
ord-2e504847da2e45d7a3f084623e24a0ac
出典データセット
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06310095B1

反応ノート

読み込み中…

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