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Sodium Hydroxide → 6-(2,4-Dichlorophenyl)-5-(4-chlorophenyl)pyridine-2-carboxylic acid

HRID 916960
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HRID 916960 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:14]=[C:13]([C:15]([O:17]C)=[O:16])[CH:12]=[CH:11][C:10]=1[C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1.[OH-].[Na+]>CO>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:14]=[C:13]([C:15]([OH:17])=[O:16])[CH:12]=[CH:11][C:10]=1[C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 10126602Methyl 6-(2,4-dichlorophenyl)-5-(4-chlorophenyl)pyridine-2-carboxylate

생성물 1

HCID 694160556-(2,4-Dichlorophenyl)-5-(4-chlorophenyl)pyridine-2-carboxylic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of methyl 6-(2,4-dichlorophenyl)-5-(4-chlorophenyl)pyridine-2-carboxylate (300 mg, 0.76 mmol) from Example 95, Step E in methanol (6 mL) was added 5N sodium hydroxide (0.300 mL, 1.5 mmol). The reaction was stirred at rt for 20 h and was then concentrated in vacuo. The residue was partitioned between methylene chloride and 2N hydrochloric acid. The organic layer was washed with brine, dried over sodium sulfate, and evaporated to give the crude title compound as a yellow foam. HPLC/MS: 378 (M+1), 380 (M+3); Rt=3.73 min

후처리

  1. concentrationwas then concentrated in vacuo
  2. customThe residue was partitioned between methylene chloride and 2N hydrochloric acid
  3. washThe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-4811587917fb4eeea48457306e25e35a
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07271266B2

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