3-Hydroxyanthranilic Acid → 2-Amino-5-bromo-3-hydroxybenzoic Acid

HRID 17512

반응식

HRID 17512 반응식
[OH:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:4]([C:5]([OH:7])=[O:6])[C:3]=1[NH2:11].[Br:12]Br.CO.O>C(O)(=O)C>[NH2:11][C:3]1[C:2]([OH:1])=[CH:10][C:9]([Br:12])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6]

참가 물질

6

반응물 4

HCID 863-Hydroxyanthranilic AcidHCID 887MethanolHCID 962WaterHCID 24408Bromine

생성물 1

HCID 217551432-Amino-5-bromo-3-hydroxybenzoic Acid수율 97%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

3-Hydroxyanthranilic acid (6.28 g, 41.0 mmol) was dissolved in acetic acid (550 ml), then a solution of bromine (13.1 g, 82.0 mmol) dissolved in acetic acid (50 ml) was gradually and dropwise added at room temperature, taking 20 minutes. After stirring at room temperature for 2.5 hours, methanol (70 ml) and water (300 ml) were added to the solution, followed by stirring at room temperature for 15 hours. The formed solid was collected by nitration, and dried under reduced pressure to obtain the entitled compound (9.129 g, 97%) as a brown powder.

후처리

  1. additiondropwise added at room temperature
  2. stirringby stirring at room temperature for 15 hours
  3. customThe formed solid was collected by nitration
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-4ad1f4d15d514ec0aa6dbe5e8378817a
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

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