Lithium Hydroxide → HCID 68816288, 화합물

HRID 1436685노트

반응식

HRID 1436685 반응식
C[O:2][C:3](=[O:26])[C:4]1[CH:16]=[C:15]([C:17]([F:25])([F:24])[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:14]=[C:6]([C:7]([N:9]([CH3:13])[CH2:10][CH2:11][CH3:12])=[O:8])[CH:5]=1.[OH-].[Li+]>C1COCC1>[F:24][C:17]([F:25])([C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[C:15]1[CH:14]=[C:6]([C:7]([N:9]([CH3:13])[CH2:10][CH2:11][CH3:12])=[O:8])[CH:5]=[C:4]([CH:16]=1)[C:3]([OH:26])=[O:2]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 68814399HCID 68814399, 화합물

생성물 1

HCID 68816288HCID 68816288, 화합물수율 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Chill a solution of 5-(difluorophenyl-methyl)-N-methyl-N-propyl-isophthalamic acid methyl ester (0.043 g, 0.119 mmol) in THF (1 mL) in an ice bath. Add 1 N lithium hydroxide (0.18 mL, 0.18 mmol) and stir at room temperature for 3 h. Acidify the solution to about pH=2 and concentrate to one half of the solvent. Partition the residue between ethyl acetate and H2O. Extract the aqueous layer with ethyl acetate (2×10 mL). Wash the combined organic extract with saturated aqueous sodium chloride, dry (magnesium sulfate) and concentrate to give the title compound (95%).

후처리

  1. concentrationconcentrate to one half of the solvent
  2. customPartition the residue between ethyl acetate and H2O
  3. extractionExtract the aqueous layer with ethyl acetate (2×10 mL)
  4. washWash the combined
  5. extractionorganic extract with saturated aqueous sodium chloride
  6. dry with materialdry (magnesium sulfate)
  7. concentrationconcentrate

출처 및 근거

ORD 기록
ord-9318eed2bca4423eb006a6eb8e82aa25
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618978B2

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