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

HRID 1517042

반응식

HRID 1517042 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 110411434-(Thiophen-3-yl)butanoic acid수율 96.1%

시약·촉매·용매 1

HCID 8150Diglyme용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b013f66cb3bf42249f49096a9bf2b275
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08227486B2

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