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Phosphorus oxychloride → 5-Benzylthiophene-2-sulfonyl chloride

HRID 1251710
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HRID 1251710 반응식
P(Cl)(Cl)(Cl)(Cl)Cl.[CH2:7]([C:14]1[S:18][C:17]([S:19]([OH:22])(=O)=[O:20])=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.P(Cl)(Cl)([Cl:25])=O>>[CH2:7]([C:14]1[S:18][C:17]([S:19]([Cl:25])(=[O:22])=[O:20])=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
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참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 22998500HCID 22998500, 화합물

생성물 1

HCID 134257165-Benzylthiophene-2-sulfonyl chloride수율 39%

실험 절차

Phosphorous pentachloride (2.08 g, 40 mmol) was added to a solution of 5-benzylthiophene-2-sulfonic acid in phosphorous oxychloride (6.0 g, 40 mmol) at 0° C. The reaction mixture was kept at 50° C. for 1 h, cooled to room temperature, then poured onto crushed ice (50 g) and extracted with ethyl acetate (2×30 ml). Removal of the solvent under reduced pressure gave a crude product, which was purified by column chromatography using 3% ethyl acetate in hexane to give 2-benzylthiophene-5-sulfonyl chloride (0.6 g, 39% yield).

후처리

  1. additionpoured
  2. extractionextracted with ethyl acetate (2×30 ml)
  3. customRemoval of the solvent under reduced pressure
  4. customgave a crude product, which
  5. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-70aa8da67d2346f6be4bea2cb39a9aa0
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06342610B2

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