Stannous chloride dihydrate → HCID 18950796、化合物

HRID 1492450ノート

反応式

HRID 1492450 の反応式
[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

参加物

5

反応物 3

HCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 18950797HCID 18950797、化合物

生成物 1

HCID 18950796HCID 18950796、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
75 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ec8a9e0a40584238a6df9f51b040b6d4
出典データセット
uspto-grants-1994_12
特許番号
US05374643

反応ノート

読み込み中…