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

HRID 841775

반응식

HRID 841775 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-ba7b74c984b54a368ce98a401e2c202e
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06369075B1

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