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Dimethylformamide → 4-Chloro-2-[[2-chloro-4-(methylsulfonyl)phenyl]amino]-benzenepropanoic acid

HRID 910870
ノート
印刷プレビュー

反応式

HRID 910870 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][CH2:7][C:8](=[O:12])[NH:9]2)=[CH:4][CH:3]=1.[H-].[Na+].[Cl:15][C:16]1[CH:37]=[C:36]([S:38]([CH3:41])(=[O:40])=[O:39])[CH:35]=[CH:34][C:17]=1OC1C=C(C(F)(F)F)C=CC=1CCC(O)=O.CN(C=[O:46])C>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][CH2:7][C:8]([OH:12])=[O:46])=[C:10]([NH:9][C:17]2[CH:34]=[CH:35][C:36]([S:38]([CH3:41])(=[O:40])=[O:39])=[CH:37][C:16]=2[Cl:15])[CH:11]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 116259773-[2-[2-Chloro-4-(methylsulfonyl)phenoxy]-4-(trifluoromethyl)phenyl]propanoic acidHCID 136907667-Chloro-1,2,3,4-tetrahydroquinolin-2-one

生成物 1

HCID 115528094-Chloro-2-[[2-chloro-4-(methylsulfonyl)phenyl]amino]-benzenepropanoic acid

反応条件

温度
90 °C

実験手順

A solution of the product from step (ii) (0.174 g) and sodium hydride (60% wt. disp. oil, 0.039 g) in DMF (10 ml) was stirred at 50° C. for 1 hour. The product from example 3 step (vi)-(vii) (0.200 g) was added and the mixture was refluxed at 90° C. for 3 hours. The mixture was partitioned between 2M sodium hydroxide and diethyl ether. The aqueous layer was acidified with 2M hydrochloric acid, extracted with ethyl acetate and the organic layer dried and concentrated under reduced pressure to give an oil. The residue was purified using RP prep HPLC. Yield 0.061 g

後処理

  1. customThe mixture was partitioned between 2M sodium hydroxide and diethyl ether
  2. extractionextracted with ethyl acetate
  3. customthe organic layer dried
  4. concentrationconcentrated under reduced pressure
  5. customto give an oil
  6. customThe residue was purified

出典と根拠

ORDレコード
ord-84c433670f8646a5be55f83af31ce6cf
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08022248B2

反応ノート

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