Water → HCID 49875538, 화합물

HRID 1465920노트

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HRID 1465920 반응식
[Br:1][C:2]1[S:6][C:5]([C:7]([OH:9])=[O:8])=[C:4]([CH3:10])[CH:3]=1.[OH-:11].[Na+].[Mn]([O-])(=O)(=O)=O.[K+].[OH2:19]>>[Br:1][C:2]1[S:6][C:5]([C:7]([OH:9])=[O:8])=[C:4]([C:10]([OH:19])=[O:11])[CH:3]=1

참가 물질

5

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 516875Potassium PermanganateHCID 181766635-Bromo-3-methylthiophene-2-carboxylic acid

생성물 1

HCID 49875538HCID 49875538, 화합물

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온도
80 °C

실험 절차

A suspension of 5-bromo-3-methyl-thiophene-2-carboxylic acid (177 g, 0.80 mol), example 1-b, and sodium hydroxide (720 g, 18 mol) in 3 L of water was heated to 80° C. Potassium permanganate (513 g, 3.25 mol) was added in 25 g portions to the warm solution over 2-3 hours. The resultant suspension was heated to reflux temperature for 2 hours and then cooled to room temperature. The solid was filtered off and washed twice with 1 N NaOH and twice with water. The aqueous solution was acidified to pH<3 with concentrated sulfuric acid. The resulting white precipitate was collected on a medium fitted glass filter, washed twice with cold water, and dried under high vacuum to produce 112 g of a white solid. MS: (−) m/z 248.91, 250.98 (M−1, 79Br/81Br)

후처리

  1. temperatureto reflux temperature for 2 hours
  2. temperaturecooled to room temperature
  3. filtrationThe solid was filtered off
  4. washwashed twice with 1 N NaOH and twice with water
  5. customThe resulting white precipitate was collected on a medium
  6. customfitted glass
  7. filtrationfilter
  8. washwashed twice with cold water
  9. customdried under high vacuum

출처 및 근거

ORD 기록
ord-2891a89acf82407c97cfab9b2a1575a0
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09000006B2

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