Tin dichloride dihydrate → HCID 178507356, 화합물

HRID 227721노트

반응식

HRID 227721 반응식
[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

참가 물질

4

반응물 2

HCID 43835034Tin dichloride dihydrateHCID 178526490HCID 178526490, 화합물

생성물 1

HCID 178507356HCID 178507356, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eeb61c366053448ca576cb419359892e
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560467B2

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