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Lithium Hydroxide → Benzoic Acid

HRID 577337
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HRID 577337 반응식
O(C1C=CC(NC2N=CN=C(N[C:22]3[CH:23]=[C:24]([CH:29]=[CH:30][CH:31]=3)[C:25]([O:27]C)=[O:26])C=2)=CC=1)C1C=CC=CC=1.[Li+].[OH-]>CO.C1COCC1.O>[C:25]([OH:27])(=[O:26])[C:24]1[CH:29]=[CH:30][CH:31]=[CH:22][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 57708324Methyl 3-(6-(4-phenoxyphenylamino)pyrimidin-4-ylamino)benzoate

생성물 1

HCID 243Benzoic Acid수율 227.5%

시약·촉매·용매 2

HCID 962Water용매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

To a stirred solution of methyl 3-(6-(4-phenoxyphenylamino)pyrimidin-4-ylamino)benzoate (0.3 g, 0.72 mmol) in methanol/THF (2/2, 4 mL) was added LiOH (0.122 g, 2.9 mmol) in H2O (4 mL) and the reaction mixture was stirred at rt for 2 h. It was concentrated under reduced pressure. the residue was diluted with water (2 mL) and was extracted with dichloromethane (5 mL). The aqueous layer was separated and was acidified with 1.5 N HCl (pH ˜5-6) to get a white precipitate, which was collected by filtration and dried under vacuum to give 34644-phenoxyphenylamino)pyrimidin-4-ylamino)benzoic acid (0.2 g 69%) as a white solid.

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후처리

  1. concentrationIt was concentrated under reduced pressure
  2. additionthe residue was diluted with water (2 mL)
  3. extractionwas extracted with dichloromethane (5 mL)
  4. customThe aqueous layer was separated
  5. customto get a white precipitate, which
  6. filtrationwas collected by filtration
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-1ffd5243c25e4cdf88c289647e234524
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040541B2

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