Stannous chloride dihydrate → HCID 178507360、化合物

HRID 56618

反応式

HRID 56618 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 178507360HCID 178507360、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-562f0edbb8da484f9e4cc5dc1fbe8a56
出典データセット
uspto-grants-2016_09
特許番号
US09434690B2

関連ノート

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