Sodium Hydroxide → 5-Chloro-4-iodo-2-methoxybenzoic acid

HRID 1070478노트

반응식

HRID 1070478 반응식
C[O:2][C:3](=[O:14])[C:4]1[CH:9]=[C:8]([Cl:10])[C:7]([I:11])=[CH:6][C:5]=1[O:12][CH3:13].[OH-].[Na+]>CO>[Cl:10][C:8]1[C:7]([I:11])=[CH:6][C:5]([O:12][CH3:13])=[C:4]([CH:9]=1)[C:3]([OH:14])=[O:2]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 69314795Methyl 5-chloro-4-iodo-2-methoxybenzoate

생성물 1

HCID 167918585-Chloro-4-iodo-2-methoxybenzoic acid수율 91.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 5-chloro-4-iodo-2-methoxy benzoic acid methyl ester of Step B (3.00 g, 9.19 mmol) and sodium hydroxide (1.10 g, 27.6 mmol) in methanol (92 mL) was refluxed for 12 hours. The reaction was cooled to room temperature and the solvent evaporated. The residue was dissolved in 1 N sodium hydroxide (75 mL), the solution washed with diethyl ether and the organic washings discarded. The aqueous phase was acidified with 2 N HCl and extracted with diethyl ether. The combined extracts were dried over anhydrous sodium sulfate, filtered and concentrated to afford the title carboxylic acid (2.64 g) as orange crystals, m.p. 150-151° C.

후처리

  1. temperaturewas refluxed for 12 hours
  2. customthe solvent evaporated
  3. dissolutionThe residue was dissolved in 1 N sodium hydroxide (75 mL)
  4. washthe solution washed with diethyl ether
  5. extractionextracted with diethyl ether
  6. dry with materialThe combined extracts were dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-49103f9fcb314fbf85fa4ff56901cce8
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903087B2

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