Stannous chloride dihydrate → HCID 18950796, 화합물

HRID 1492450노트

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HRID 1492450 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:11]=[N:12][O:13][CH:14]=2)=[CH:6][CH:5]=1)([O-])=O.O.O.Cl[Sn]Cl.C([O-])(O)=O.[Na+]>C(OCC)(=O)C>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([C:10]2[N:11]=[N:12][O:13][CH:14]=2)=[CH:8][CH:9]=1

참가 물질

5

반응물 3

HCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 18950797HCID 18950797, 화합물

생성물 1

HCID 18950796HCID 18950796, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
75 °C

실험 절차

A mixture of 4-nitrophenyloxadiazole (2.87 g, 0.015 mol, prepared according to Lin et al., J. Org. Chem., 1979, 44, 4160) and SnCl2.2H2O (16.92 g, 0.075 mol) in 75 mL of ethyl acetate was heated at 75° C. for 30 minutes. The yellow reaction mixture was cooled to room temperature, poured into ice-water and the pH was made slightly basic (pH 7-8) by the addition of 5% NaHCO3. The reaction mixture was then extracted with ethyl acetate, dried over MgSO4 and concentrated in vacuo. The remaining yellow solid was triturated with hexane, collected and dried to yield 2.07 g of the title A compound, m.p. 97°-99° C. TLC, silica gel, EtOAc/hexanes (2:1), Rf =0.55; M.S. (M+H)+ at 162, M.W. 161. This compound was used without further purification.

후처리

  1. temperatureThe yellow reaction mixture was cooled to room temperature
  2. extractionThe reaction mixture was then extracted with ethyl acetate
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe remaining yellow solid was triturated with hexane
  6. customcollected
  7. customdried
  8. customto yield 2.07 g of the title A compound, m.p. 97°-99° C
  9. customThis compound was used without further purification

출처 및 근거

ORD 기록
ord-ec8a9e0a40584238a6df9f51b040b6d4
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05374643

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