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1-(3,5-Dioxapiperidin-1-yl)sulphonyl-4-nitrobenzene → 4-(3,5-Dioxapiperidin-1-yl)sulphonylaniline

HRID 23918
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HRID 23918 반응식
[N:1]1([S:7]([C:10]2[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[CH:12][CH:11]=2)(=[O:9])=[O:8])[CH2:6][O:5][CH2:4][O:3][CH2:2]1>[Pd].C(O)C.C(OCC)(=O)C>[N:1]1([S:7]([C:10]2[CH:15]=[CH:14][C:13]([NH2:16])=[CH:12][CH:11]=2)(=[O:8])=[O:9])[CH2:2][O:3][CH2:4][O:5][CH2:6]1
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참가 물질

5

반응물 1

HCID 220249211-(3,5-Dioxapiperidin-1-yl)sulphonyl-4-nitrobenzene

생성물 1

HCID 225702274-(3,5-Dioxapiperidin-1-yl)sulphonylaniline수율 88.9%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 1-(3,5-dioxapiperidin-1-yl)sulphonyl-4-nitrobenzene (Method 8) (500 mg, 1.82 mmol) and 10% palladium on charcoal catalyst (150 mg) in ethanol (25 ml) and ethyl acetate (25 ml) was stirred under an atmosphere of hydrogen for 3 hours. The catalyst was removed by filtration through diatomaceous earth and the filter pad was washed with ethanol and ethyl acetate. The volatiles were removed from the filtrate by evaporation and the residue triturated with ether and hexane to give the tide compound (395 mg, 88%). NMR: 4.90 (s, 2H) 5.10 (s, 4H), 6.02 (s, 2H), 6.58 (d, 2H), 7.50 (d, 2H).

후처리

  1. customThe catalyst was removed by filtration through diatomaceous earth
  2. washthe filter pad was washed with ethanol and ethyl acetate
  3. customThe volatiles were removed from the filtrate by evaporation
  4. customthe residue triturated with ether and hexane

출처 및 근거

ORD 기록
ord-ea10996620524120b6e6ff7aa80b2e1c
출처 데이터셋
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06855719B1

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