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Potassium Hydroxide → HCID 70855553, 화합물

HRID 591034
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HRID 591034 반응식
[Br:1][C:2]1[C:3]2[C:15]([CH3:16])=[CH:14][CH:13]=[CH:12][C:4]=2[S:5][C:6]=1[C:7]([O:9]CC)=[O:8].[OH-].[K+]>CO.O>[Br:1][C:2]1[C:3]2[C:15]([CH3:16])=[CH:14][CH:13]=[CH:12][C:4]=2[S:5][C:6]=1[C:7]([OH:9])=[O:8]
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참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 70855544HCID 70855544, 화합물

생성물 1

HCID 70855553HCID 70855553, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
70 °C

실험 절차

A solution of ethyl 3-bromo-4-methyl-benzo[b]thiophene-2-carboxylate (23b) (640 mg, 2.14 mmol) and potassium hydroxide (1.17 g, 21 mmol) in a mixture of methanol (10 mL) and water (5 mL) was warmed at 70° C. After 1 hour, methanol was evaporated and water (10 mL) was added to the reaction mixture which was washed with diethyl ether (10 mL). The aqueous layer was acidified to pH 2 with a hydrochloric acid solution 1N and extracted with ethyl acetate (2×10 mL). The organic layer was washed with brine (10 mL), dried over sodium sulfate, filtered and evaporated under reduced pressure to afford the desired acid (23c) as a white solid without further purification (420 mg, 1.55 mmol, 72%).

후처리

  1. custommethanol was evaporated
  2. additionwater (10 mL) was added to the reaction mixture which
  3. washwas washed with diethyl ether (10 mL)
  4. extractionextracted with ethyl acetate (2×10 mL)
  5. washThe organic layer was washed with brine (10 mL)
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-579afc84a2f9472e82cd5ddf5868f98c
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09238026B2

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