Piperidine → Piperidine-1-sulfonyl chloride

반응식

[S:1]([Cl:5])(Cl)(=[O:3])=[O:2].[NH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1>>[N:6]1([S:1]([Cl:5])(=[O:3])=[O:2])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1

참가 물질

반응물 2

HCID 8082Piperidine

HCID 24648Sulfuryl chloride

생성물 1

HCID 11298344Piperidine-1-sulfonyl chloride수율 36.3%

반응 조건

온도: 0 °C

실험 절차

A solution of sulfuryl chloride (1N in dichloromethane, 75 mL, 75 mmol) at −20° C. was treated dropwise with piperidine (12.6 g, 150 mmol), stirred at 0° C. for 2 hours, and partitioned between dichloromethane and water (50 mL). The organic layer was washed with aqueous 1N HCl, brine and dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was distilled under reduced pressure (1 mm Hg) at 105° C. to give the title compound (5 grams).

후처리

custompartitioned between dichloromethane and water (50 mL)
washThe organic layer was washed with aqueous 1N HCl, brine
dry with materialdried over anhydrous magnesium sulfate
filtrationfiltered
concentrationconcentrated under reduced pressure
distillationThe residue was distilled under reduced pressure (1 mm Hg) at 105° C.

출처 및 근거

ORD 기록: ord-42a00bc52f6140398ccdc6b6f995e306
출처 데이터셋: uspto-grants-2011_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07902203B2

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