Acetic Acid → HCID 14404122, 화합물

HRID 465506노트

반응식

HRID 465506 반응식
C(OO)(=[O:3])C.C(O)(=O)C.[CH:10]1[C:23]2[CH:22]=[C:21]([S:24][CH2:25][N+:26]([O-:28])=[O:27])[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]=2[CH:13]=[CH:12][CH:11]=1.[OH2:29]>C(Cl)(Cl)Cl>[CH:10]1[C:23]2[CH:22]=[C:21]([S:24]([CH2:25][N+:26]([O-:28])=[O:27])(=[O:3])=[O:29])[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]=2[CH:13]=[CH:12][CH:11]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 6585Peracetic AcidHCID 14404129HCID 14404129, 화합물

생성물 1

HCID 14404122HCID 14404122, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of peracetic acid in acetic acid (32 wt%, 4 ml, 19 mmol) was added dropwise to an efficiently stirred solution of (9-phenanthrylthio)nitromethane (A) (1 g, 3.7 mmol) in chloroform (50 ml). The mixture was stirred for 20 hours and then diluted with water (20 ml). The organic phase was separated and washed with an aqueous solution of sodium metabisulphite, then with brine, and dried (N2SO4). The solvent was removed by evaporation to give a yellow solid. This was purified by flash chromatography on silica (Merck Kieselgel Art. 7736) eluting with toluene to give (9-phenanthrylsulphonyl)nitromethane, as a white crystalline solid (180 mg, 16% yield) m.p. 165°-166° C., (after recrystallisation from toluene); microanalysis, found: C, 59.7; H, 3.7; N, 4.6%; C15H11NO4S requires: C, 59.8; H, 3.7; N, 4.7%

후처리

  1. customThe organic phase was separated
  2. washwashed with an aqueous solution of sodium metabisulphite
  3. dry with materialwith brine, and dried (N2SO4)
  4. customThe solvent was removed by evaporation
  5. customto give a yellow solid
  6. customThis was purified by flash chromatography on silica (Merck Kieselgel Art. 7736)
  7. washeluting with toluene

출처 및 근거

ORD 기록
ord-1fa46703b2dc4189b4116656b6db1258
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05153227

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