Ammonium Hydroxide → 4-(Thiophen-3-yl)butanoic acid

HRID 1517042

反応式

HRID 1517042 の反応式
[S:1]1[CH:5]=[CH:4][C:3]([CH2:6][CH2:7][CH:8](C(O)=O)[C:9]([OH:11])=[O:10])=[CH:2]1.[OH-].[NH4+]>COCCOCCOC>[S:1]1[CH:5]=[CH:4][C:3]([CH2:6][CH2:7][CH2:8][C:9]([OH:11])=[O:10])=[CH:2]1

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 54550536[2-(Thiophen-3-yl)ethyl]propanedioic acid

生成物 1

HCID 110411434-(Thiophen-3-yl)butanoic acid収率 96.1%

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

実験手順

The product from Step C (2.4 g, 11.0 mmol) was dissolved in 2-methoxyethyl ether (20 mL) and refluxed for 24 hours. The reaction was cooled to room temperature and basified to pH 9 with concentrated ammonium hydroxide. The mixture was extracted once with diethyl ether and set aside. The aqueous layer was acidified with concentrated hydrochloride acid and extracted four times with diethyl ether. The extract were combined and dried over sodium sulfate, filtered and concentrated to give 4-thiophen-3-yl-butyric acid (1.8 g, 95%) as an oil.

後処理

  1. temperaturerefluxed for 24 hours
  2. extractionThe mixture was extracted once with diethyl ether
  3. extractionextracted four times with diethyl ether
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-b013f66cb3bf42249f49096a9bf2b275
出典データセット
uspto-grants-2012_07
特許番号
US08227486B2

関連ノート

読み込み中…