Hydrochloric Acid → HCID 69001756、化合物

HRID 1821317ノート

反応式

HRID 1821317 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1/[CH:10]=[CH:11]/[C:12]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[NH:14][N:13]=1)([O-])=O.[Sn].Cl.[OH-].[Na+]>C(O)C>[NH:14]1[C:15]2[C:20](=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:12](/[CH:11]=[CH:10]/[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[NH2:1])=[N:13]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 5352426Tin atomHCID 68999900(E)-3-[2-(2-nitrophenyl)vinyl]-1H-indazole

生成物 1

HCID 69001756HCID 69001756、化合物収率 84%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

(E)-3-[2-(2-nitrophenyl)vinyl]-1H-indazole (4 g, 15.08 mmol) obtained in Example 1 was dissolved in ethanol (68 mL), and the solution was added with tin (3.85 g, 32.40 mmol) and concentrated hydrochloric acid (34 mL, 400 mmol) under ice-cooling, followed by stirring at 40° C. for 3 hours. To the reaction mixture, 6 mol/L aqueous sodium hydroxide solution was added to neutralize the mixture under ice-cooling. Then the mixture was filtered. The filtrate was added with saturated aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and then the solvent was evaporated under reduced pressure. The residue was triturated in ethyl acetate to obtain Compound 2 (2.98 g, 84%).

後処理

  1. temperaturecooling
  2. temperaturecooling
  3. filtrationThen the mixture was filtered
  4. additionThe filtrate was added with saturated aqueous sodium hydrogencarbonate solution
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with water and saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customthe solvent was evaporated under reduced pressure
  9. customThe residue was triturated in ethyl acetate

出典と根拠

ORDレコード
ord-1945d9d85449493e9e5d16ae1e177062
出典データセット
uspto-grants-2009_10
特許番号
US07605272B2

反応ノート

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