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

HRID 448892노트

반응식

HRID 448892 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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)

후처리

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

출처 및 근거

ORD 기록
ord-557ab0bb7e8d43a8bb027eee811221a7
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481738B2

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