Carbon Dioxide → 4-Bromo-3-thenoic acid

HRID 368671

反応式

HRID 368671 の反応式
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

参加物

6

反応物 3

HCID 280Carbon DioxideHCID 184523,4-DibromothiopheneHCID 178418306HCID 178418306、化合物

生成物 1

HCID 855464-Bromo-3-thenoic acid収率 70.3%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8003Pentane溶媒

反応条件

温度
-78 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-6212e6e68c5b487ea0df8610456e50d7
出典データセット
uspto-grants-2000_10
特許番号
US06133252

関連ノート

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