Carbon Dioxide → 4-Bromo-3-thenoic acid

HRID 368671

반응식

HRID 368671 반응식
Br[C:2]1[C:6]([Br:7])=[CH:5][S:4][CH:3]=1.[Li]C(C)(C)C.[C:13](=[O:15])=[O:14]>CCOCC.CCCCC>[Br:7][C:6]1[C:2]([C:13]([OH:15])=[O:14])=[CH:3][S:4][CH:5]=1

참가 물질

6

반응물 3

HCID 280Carbon DioxideHCID 184523,4-DibromothiopheneHCID 178418306HCID 178418306, 화합물

생성물 1

HCID 855464-Bromo-3-thenoic acid수율 70.3%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8003Pentane용매

반응 조건

온도
-78 °C

실험 절차

To a solution of 3,4-dibromothiophene (15 g, 62 mmol) in 80 mL ether under a positive nitrogen atmosphere was added dropwise 75 mL 1.7M t-BuLi in pentane at below -73° C. and the resulting reaction solution was stirred at -78° C. for 0.5 h. After that, the ether solution was poured into dry ice and extracted with water. The aq solution was washed with ether and then acidified with concentrated HCl. The solid was filtered and air-dried to give 9 g of 4-bromo-3-thiophenecarboxylic acid, yield 70.3%.

후처리

  1. customthe resulting reaction solution
  2. extractionextracted with water
  3. washThe aq solution was washed with ether
  4. filtrationThe solid was filtered
  5. customair-dried

출처 및 근거

ORD 기록
ord-6212e6e68c5b487ea0df8610456e50d7
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06133252

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