Stannous chloride dihydrate → HCID 178507360, 화합물

HRID 56618

반응식

HRID 56618 반응식
[Cl: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.O.O.[Sn](Cl)Cl.C(=O)(O)[O-].[Na+]>C(O)C>[NH2:11][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][CH:7]=1)[NH:4][N:3]=[C:2]2[Cl:1]

참가 물질

5

반응물 3

HCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 1785264933-Chloro-5-nitro-1H-indazole

생성물 1

HCID 178507360HCID 178507360, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.00 g (5.06 mmol) of 3-chloro-5-nitro-1H-indazole was suspended in 50 ml of ethanol, and 5.71 g (25.3 mmol) of tin(II) chloride dihydrate were added. The mixture was left to stir at reflux overnight, saturated aqueous sodium bicarbonate solution was then added and the mixture was extracted three times with ethyl acetate. The combined organic phases were dried over magnesium sulphate and the solvent was removed under reduced pressure. The mixture was triturated with tert-butyl methyl ether and the solid was filtered off with suction. Yield: 544 mg (purity 90%, 58% of theory)

후처리

  1. waitThe mixture was left
  2. temperatureat reflux overnight
  3. extractionthe mixture was extracted three times with ethyl acetate
  4. dry with materialThe combined organic phases were dried over magnesium sulphate
  5. customthe solvent was removed under reduced pressure
  6. customThe mixture was triturated with tert-butyl methyl ether
  7. filtrationthe solid was filtered off with suction

출처 및 근거

ORD 기록
ord-562f0edbb8da484f9e4cc5dc1fbe8a56
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434690B2

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