Lithium hydroxide, monohydrate → 2-(5-(Trifluoromethyl)pyridin-2-yl)benzoic acid

HRID 51912

반응식

HRID 51912 반응식
C([O:4][C:5](=[O:22])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12]1[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][N:13]=1)(C)C.O.[OH-].[Li+]>O1CCCC1CO.O>[F:20][C:18]([F:19])([F:21])[C:15]1[CH:16]=[CH:17][C:12]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]([OH:22])=[O:4])=[N:13][CH:14]=1

참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 698912952-(5-Trifluoromethyl-pyridin-2-yl)-benzoic acid isopropyl ester

생성물 1

HCID 227369092-(5-(Trifluoromethyl)pyridin-2-yl)benzoic acid

시약·촉매·용매 1

HCID 66577907Tetrahydrofuran-methanol water용매

실험 절차

2-(5-Trifluoromethyl-pyridin-2-yl)-benzoic acid isopropyl ester was dissolved in 10 ml of a 3:1:1 mixture of tetrahydrofuran-methanol-water, and lithium hydroxide monohydrate (161 mg, 3.84 mmol) was added. After stirring for 3 h at room temperature, the volatiles were removed under vacuum and 5 ml of water were added to the mixture, which was brought to pH 6 with 1N HCl. The resulting slurry was extracted with ethyl acetate, the combined organic layers were dried (magnesium sulfate), filtered and concentrated under vacuum to provide the title compound.

후처리

  1. additionwas added
  2. customthe volatiles were removed under vacuum and 5 ml of water
  3. additionwere added to the mixture, which
  4. extractionThe resulting slurry was extracted with ethyl acetate
  5. dry with materialthe combined organic layers were dried (magnesium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-15d651bafd9244f8b7ddf9e9319aa1c2
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06713489B2

연결된 노트

불러오는 중…