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Phosphorus pentachloride → HCID 59623758, 화합물

HRID 1093942
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반응식

HRID 1093942 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[CH2:12][S:13]([OH:16])(=O)=[O:14].[Na].P(Cl)(Cl)(Cl)(Cl)[Cl:19]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[CH2:12][S:13]([Cl:19])(=[O:16])=[O:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24819Phosphorus pentachlorideHCID 87086675HCID 87086675, 화합물

생성물 1

HCID 59623758HCID 59623758, 화합물수율 91.6%

반응 조건

온도
85 °C

실험 절차

A mixture of sodium (2-chloro-5-trifluoromethyl-phenyl)-methanesulfonic acid (Example 1.1) (9.4 g) and phosphorous pentachloride (13.5 g) was heated to 80-90° C. for 4 hours. The reaction mixture was concentrated. The residue was poured onto a mixture of ice and water and the mixture extracted twice with dichloromethane. The combined organic extracts were washed with water and brine, dried over magnesium sulfate and concentrated to give (2-chloro-5-trifluoromethyl-phenyl)-methanesulfonyl chloride as an off-white solid (8.480 g). 1H-NMR (400 MHz, CDCl3): 7.87 (m, 1H), 7.68 (m, 2H), 5.15 (s, 2H) ppm.

후처리

  • concentrationThe reaction mixture was concentrated
  • additionThe residue was poured onto a mixture of ice and water
  • extractionthe mixture extracted twice with dichloromethane
  • washThe combined organic extracts were washed with water and brine
  • dry with materialdried over magnesium sulfate
  • concentrationconcentrated
  • 출처 및 근거

    ORD 기록
    ord-f80b9ea278394e7593b106a810eb1dc1
    출처 데이터셋
    uspto-grants-2012_03
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08133849B2

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