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Hydrochloric Acid → N-(3-(1-Chloro-2-nitroethenylthio)propyl)benzenesulfonamide

HRID 364861
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HRID 364861 반응식
[OH-].[Na+].[SH:3][CH2:4][CH2:5][CH2:6][NH:7][S:8]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)(=[O:10])=[O:9].[Cl:17][C:18](Cl)=[CH:19][N+:20]([O-:22])=[O:21].Cl.[Cl-].[Na+]>CO>[Cl:17][C:18]([S:3][CH2:4][CH2:5][CH2:6][NH:7][S:8]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)(=[O:10])=[O:9])=[CH:19][N+:20]([O-:22])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 122195711,1-Dichloro-2-nitroetheneHCID 20238482N-(3-Mercaptopropyl)benzenesulfonamide

생성물 1

HCID 54130017N-(3-(1-Chloro-2-nitroethenylthio)propyl)benzenesulfonamide

시약·촉매·용매 1

HCID 887Methanol용매3회

실험 절차

A solution of 0.08 g of sodium hydroxide in 3 ml of methanol was added drop-by-drop over 5 minutes to a solution of 0.23 g of 3 in 5 ml of methanol. The resulting mixture was added drop-by-drop over 20 minutes to a solution of 0.28 g of 13A in 6 ml of methanol at 0° C. The mixture was held at 0° C. for 30 minutes, then poured into 2% hydrochloric acid saturated with sodium chloride. The resulting mixture was extracted with methylene chloride, the solvent was evaporated from the extract and the residue was chromatographed over silica gel to give 14, as a solid, m.p.: 105°-106° C.

후처리

  1. extractionThe resulting mixture was extracted with methylene chloride
  2. customthe solvent was evaporated from the
  3. extractionextract
  4. customthe residue was chromatographed over silica gel

출처 및 근거

ORD 기록
ord-0f69d14c4db346b98b08abc54d58fad2
출처 데이터셋
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04606862

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