Phosphorus pentachloride → heptane-1-sulfonyl chloride

반응식

P(Cl)(Cl)(Cl)(Cl)[Cl:2].[CH2:7]([S:14]([OH:17])(=O)=[O:15])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].[Na]>>[CH2:7]([S:14]([Cl:2])(=[O:17])=[O:15])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

참가 물질

반응물 3

HCID 24819Phosphorus pentachloride

HCID 898291-Heptanesulfonic acid

HCID 5360545Sodium

생성물 1

HCID 10878141heptane-1-sulfonyl chloride

실험 절차

To phosphorous pentachloride (3.3 g, 16 mmol) was added solid heptanesulfonic acid, sodium salt monohydrate (1.75 g, 8 mmol) and the mixture was left to stir overnight under nitrogen. Phosphorous oxychloride was removed by distillation at 150° C. for 3 h. The residue was distilled under reduced pressure (ca. 5 mm Hg) at 135° C. to give ca. 1 g of material which was allowed to cool to room temperature. The precipitated free acid was removed by filtration to afford the title compound as an oil (500 mg, 31%) which was used without further purification.

후처리

waitthe mixture was left
customPhosphorous oxychloride was removed by distillation at 150° C. for 3 h
distillationThe residue was distilled under reduced pressure (ca. 5 mm Hg) at 135° C.

출처 및 근거

ORD 기록: ord-99f74e0b64e84e4dad4737a1816ed3d2
출처 데이터셋: uspto-grants-2003_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06610711B2

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