Sodium Hydroxide → 4-Methylthiophene-2-carboxylic acid

HRID 2377249

반응식

HRID 2377249 반응식
Cl[O-:2].[Na+].[OH-].[Na+].[C:6]([C:9]1[S:10][CH:11]=[C:12]([CH3:14])[CH:13]=1)(=[O:8])C>>[CH3:14][C:12]1[CH:13]=[C:9]([C:6]([OH:8])=[O:2])[S:10][CH:11]=1

참가 물질

4

반응물 3

HCID 14798Sodium Hydroxide2회HCID 836541-(4-Methyl-2-thienyl)ethan-1-oneHCID 23665760Sodium Hypochlorite

생성물 1

HCID 27945844-Methylthiophene-2-carboxylic acid

반응 조건

온도
70 °C

실험 절차

To an aqueous solution of sodium hypochlorite (available chlorine 5%) (92.6 mL, 143.0 mmol) at about 0° C. was added sodium hydroxide (1.14 g, 28.6 mmol) and the mixture was stirred at about 0° C. until all of the sodium hydroxide had dissolved. To this solution was added 2-acetyl-4-methylthiophene (2.0 g, 14.3 mmol) at about 0° C. After the addition was complete, the mixture was heated to about 70° C. for about 3 hours, then the solution was cooled and was carefully quenched by addition of a solution of sodium bisulfite (23 g) in water (150 mL). After stirring for about 20 minutes, the solution was acidified by addition of concentrated hydrochloric acid and the precipitate was collected by filtration and dried under high vacuum to provide the desired product. MS (DCI-NH3): m/z 160 (M+NH4)+.

후처리

  1. dissolutionhad dissolved
  2. additionAfter the addition
  3. temperaturethe solution was cooled
  4. customwas carefully quenched by addition of a solution of sodium bisulfite (23 g) in water (150 mL)
  5. additionthe solution was acidified by addition of concentrated hydrochloric acid
  6. filtrationthe precipitate was collected by filtration
  7. customdried under high vacuum

출처 및 근거

ORD 기록
ord-3f94701b2fcd4e8ba9d9f32f00cecf91
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07468371B2

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