Tin dichloride dihydrate → HCID 178507356、化合物

HRID 227721ノート

反応式

HRID 227721 の反応式
[Br:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([N+:11]([O-])=O)[CH:9]=2)[NH:4][N:3]=1.Cl[Sn]Cl.O>CCO>[Br:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([NH2:11])[CH:9]=2)[NH:4][N:3]=1

参加物

4

反応物 2

HCID 43835034Tin dichloride dihydrateHCID 178526490HCID 178526490、化合物

生成物 1

HCID 178507356HCID 178507356、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The product of Step (a) (10.0 g, 41.3 mmol, 1.00 equiv) was suspended in EtOH (120 mL). SnCl2.H2O (46.6 g, 206 mmol, 5.00 equiv) was added and the mixture was refluxed for 18 hours. The reaction mixture was concentrated en vacuo and water was added to the residue. The mixture was basified to pH 8 with satd. NaHCO3 and extracted with EtOAc (3×). The combined organic extracts were washed with satd. NaCl, dried over MgSO4, filtered and concentrated en vacuo. 8.10 g (92%) of the title compound was iolated as a purple solid.

後処理

  1. temperaturethe mixture was refluxed for 18 hours
  2. concentrationThe reaction mixture was concentrated en vacuo and water
  3. additionwas added to the residue
  4. extractionNaHCO3 and extracted with EtOAc (3×)
  5. washThe combined organic extracts were washed with satd
  6. dry with materialNaCl, dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated en vacuo

出典と根拠

ORDレコード
ord-eeb61c366053448ca576cb419359892e
出典データセット
uspto-grants-2009_07
特許番号
US07560467B2

反応ノート

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