Hydrochloric Acid → 3-(1-{1-[(4-Chlorophenyl)(3-cyanophenyl)methyl]azetidin-3-yl}-2-fluoro-2-methylpropyl)-5-fluorobenzoic acid

HRID 602991노트

반응식

HRID 602991 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([C:36]#[N:37])[CH:31]=2)[N:9]2[CH2:12][CH:11]([CH:13]([C:18]3[CH:19]=[C:20]([CH:26]=[C:27]([F:29])[CH:28]=3)[C:21]([O:23]CC)=[O:22])[C:14]([F:17])([CH3:16])[CH3:15])[CH2:10]2)=[CH:4][CH:3]=1.[Li+].[OH-].Cl>CCO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([C:36]#[N:37])[CH:31]=2)[N:9]2[CH2:12][CH:11]([CH:13]([C:18]3[CH:19]=[C:20]([CH:26]=[C:27]([F:29])[CH:28]=3)[C:21]([OH:23])=[O:22])[C:14]([F:17])([CH3:16])[CH3:15])[CH2:10]2)=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 67055325HCID 67055325, 화합물

생성물 1

HCID 670553863-(1-{1-[(4-Chlorophenyl)(3-cyanophenyl)methyl]azetidin-3-yl}-2-fluoro-2-methylpropyl)-5-fluorobenzoic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 112 mg (0.214 mmol) of ethyl 3-(1-{1-[(4-chlorophenyl)(3-cyanophenyl)methyl]azetidin-3-yl}-2-fluoro-2-methylpropyl)-5-fluorobenzoate and 1.2 mL of 1M LiOH in 5 mL of EtOH was stirred for 2.5 h at rt. The solution was adjusted to pH=5-6 with 6N HCl and concentrated to remove solvents. The residue was dissolve in 10 mL of CH2Cl2 and solids were removed by filtration. The solution was concentrated to afford the title compound as a white solid; Mass Spectrum: m/e=495 (M+1, 35Cl), 497 (M+1, 37Cl).

후처리

  1. concentrationconcentrated
  2. customto remove solvents
  3. dissolutionThe residue was dissolve in 10 mL of CH2Cl2
  4. customsolids were removed by filtration
  5. concentrationThe solution was concentrated

출처 및 근거

ORD 기록
ord-034f6d11a58b44c0ab27c4f78b25ebd7
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906652B2

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