Tetrahydrofuran → 4-Chloro-3-(3,5-dichloro-pyridin-2-yl)-benzoic acid

HRID 1485960ノート

反応式

HRID 1485960 の反応式
C1COCC1.C[O:7][C:8](=[O:24])[C:9]1[CH:14]=[CH:13][C:12]([Cl:15])=[C:11]([C:16]2[C:21]([Cl:22])=[CH:20][C:19]([Cl:23])=[CH:18][N:17]=2)[CH:10]=1.O[Li].O>O>[Cl:15][C:12]1[CH:13]=[CH:14][C:9]([C:8]([OH:24])=[O:7])=[CH:10][C:11]=1[C:16]1[C:21]([Cl:22])=[CH:20][C:19]([Cl:23])=[CH:18][N:17]=1

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 686021224-Chloro-3-(3,5-dichloro-pyridin-2-yl)-benzoic acid methyl ester

生成物 1

HCID 686040024-Chloro-3-(3,5-dichloro-pyridin-2-yl)-benzoic acid収率 85.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of THF (15 mL) and water (1 mL) containing 4-chloro-3-(3,5-dichloro-pyridin-2-yl)-benzoic acid methyl ester (1.7 g, 5.4 mmol) and LiOH.H2O (0.68 g, 16.1 mmol) was stirred at room temperature for 12 hrs. The mixture was acidified and extracted with ethyl acetate. The organic layer was washed with brine and water and was dried. Filtration and concentration gave 4-chloro-3-(3,5-dichloro-pyridin-2-yl)-benzoic acid as a white solid (1.4 g). MS (M+H)+: 301.6, tR=7.048 min (method 2)

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine and water
  3. customwas dried
  4. filtrationFiltration and concentration

出典と根拠

ORDレコード
ord-8d7e8410eb6c4160b249e16117c86378
出典データセット
uspto-grants-2016_08
特許番号
US09422310B2

反応ノート

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