Sodium Hydroxide → HCID 178435087, 화합물

HRID 2298690노트

반응식

HRID 2298690 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:8]([O:10]C)=[S:9])[S:5][C:6]=1[CH3:7].[OH-].[Na+]>CO.O>[Br:1][C:2]1[CH:3]=[C:4]([C:8]([OH:10])=[S:9])[S:5][C:6]=1[CH3:7]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 86583861Methyl 4-bromo-5-methylthiothiophene-2-carboxylate

생성물 1

HCID 178435087HCID 178435087, 화합물수율 94.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To 1.0 g (3.7 mmol) of methyl 4-bromo-5-methylthiothiophene-2-carboxylate (as prepared in Example 241, step (a) dissolved in 25 ml of MeOH was added 450 mg of NaOH dissolved in 10 ml of H2O. The reaction was stirred for 5 hours at room temperature, and then the solvents were removed under vacuum. The residue of the reaction was extracted with ethyl acetate (2×50 mL) and 1N HCl. The organic layer was collected, dried (Na2SO4), filtered and concentrated under vacuum to yield 833 mg (89%) of 4-bromo-5-methylthiothiophene-2-carboxylic acid as a white solid.

후처리

  1. customthe solvents were removed under vacuum
  2. extractionThe residue of the reaction was extracted with ethyl acetate (2×50 mL) and 1N HCl
  3. customThe organic layer was collected
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-cfb4b2fe0a3e4295bf63c692cff55db8
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06492403B1

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