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Water → Ethyl 2-isopropoxy-3-[4-methoxy-3-({[2-fluoro-4-(trifluoromethyl)benzoyl]amino}methyl)phenyl]propanoate

HRID 1816573
ノート
印刷プレビュー

反応式

HRID 1816573 の反応式
[NH2:1][CH2:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([O:18][CH:19]([CH3:21])[CH3:20])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].N1C=CC=CC=1.[Cl-].[F:29][C:30]1[CH:38]=[C:37]([C:39]([F:42])([F:41])[F:40])[CH:36]=[CH:35][C:31]=1[C:32]([O-])=[O:33].O>CN(C)C=O>[CH:19]([O:18][CH:12]([CH2:11][C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([CH2:2][NH:1][C:32](=[O:33])[C:31]2[CH:35]=[CH:36][C:37]([C:39]([F:40])([F:41])[F:42])=[CH:38][C:30]=2[F:29])[CH:4]=1)[C:13]([O:15][CH2:16][CH3:17])=[O:14])([CH3:20])[CH3:21]
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 962WaterHCID 1049PyridineHCID 22493983Ethyl 3-[3-(aminomethyl)-4-methoxyphenyl]-2-isopropoxypropanoateHCID 224942742-Fluoro-4-(trifluoromethyl)benzoate chloride

生成物 1

HCID 22493991Ethyl 2-isopropoxy-3-[4-methoxy-3-({[2-fluoro-4-(trifluoromethyl)benzoyl]amino}methyl)phenyl]propanoate収率 81.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.15 g of ethyl 3-[3-(aminomethyl)-4-methoxyphenyl]-2-isopropoxypropanoate was dissolved in 5 ml N,N-dimethylformamide, and 0.2 ml pyridine and 0.24 g of 2-fluoro-4-(trifluoromethyl)benzoate chloride were added, followed by stirring at room temperature for 12 hours. Water was added to the reaction solution, followed by extracting with ethyl acetate The extract was washed with brine, dried over anhydrous magnesium sulfate and the solvent was evapoarated. The residue was subjected to silica gel column chromatography, and from fractions eluted with ethyl acetate-hexane (1:2), 0.2 g of ethyl 2-isopropoxy-3-[4-methoxy-3-({[2-fluoro-4-(trifluoromethyl)benzoyl]amino}methyl)phenyl]propanoate was obtained as a pale yellow oil. This product was treated in the same manner as in Example 1d), to give 0.15 g of 2-isopropoxy-3-[4-methoxy-3-{[2-fluoro-4-(trifluoromethyl)benzoyl]amino}methyl)phenyl]propanoic acid as a pale yellow solid.

後処理

  1. extractionby extracting with ethyl acetate The extract
  2. washwas washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. washfrom fractions eluted with ethyl acetate-hexane (1:2)

出典と根拠

ORDレコード
ord-ef68cc2d2d64433caca4d80357893d57
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06884821B1

反応ノート

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