Bromine → Methyl 4-bromo-3-hydroxy-5-methylthiophene-2-carboxylate

HRID 621784노트

반응식

HRID 621784 반응식
[Br:1]Br.[OH:3][C:4]1[CH:8]=[C:7]([CH3:9])[S:6][C:5]=1[C:10]([O:12][CH3:13])=[O:11]>C(O)(=O)C>[Br:1][C:8]1[C:4]([OH:3])=[C:5]([C:10]([O:12][CH3:13])=[O:11])[S:6][C:7]=1[CH3:9]

참가 물질

4

반응물 2

HCID 24408BromineHCID 587860Methyl 3-hydroxy-5-methylthiophene-2-carboxylate

생성물 1

HCID 54697143Methyl 4-bromo-3-hydroxy-5-methylthiophene-2-carboxylate수율 56.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Bromine (4.6 g, 29 mmoles) is added dropwise at room temperature to a stirred solution of methyl 3-hydroxy-5-methyl-2-thiophenecarboxylate (5.0 g, 29 mmoles) in acetic acid (25 mL). After 16 hours the mixture is stirred into ice water (200 mL), and the precipitate is filtered off, rinsed with water, with aqueous sodium thiosulfate, again with water and dried. Recrystallization from methyl t-butyl ether gave the pure product (4.1 g); mp 96°-97° C.

후처리

  1. filtrationthe precipitate is filtered off
  2. washrinsed with water, with aqueous sodium thiosulfate, again with water
  3. customdried
  4. customRecrystallization from methyl t-butyl ether

출처 및 근거

ORD 기록
ord-8b9cadf2f66d47da880a6a4c28ed3489
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824958

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