Hydrochloric Acid → HCID 178468965、化合物

HRID 82022ノート

反応式

HRID 82022 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:7]2[CH:15]=[N:14][NH:13][C:8]=2[N:9]=[C:10]([Cl:12])[CH:11]=1)=[O:5])[CH3:2].C(=O)([O-])O.[Na+].[I:21]I.S([O-])([O-])(=O)=S.[Na+].[Na+].Cl>O1CCOCC1>[CH2:1]([O:3][C:4]([C:6]1[C:7]2[C:15]([I:21])=[N:14][NH:13][C:8]=2[N:9]=[C:10]([Cl:12])[CH:11]=1)=[O:5])[CH3:2]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 807Iodine2 回HCID 24477Sodium ThiosulfateHCID 516892Sodium BicarbonateHCID 86678157ethyl 6-chloro-1H-pyrazolo(3,4-b)pyridine-4-carboxylate

生成物 1

HCID 178468965HCID 178468965、化合物収率 95%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

In a 1 L single necked flask were charged 6-chloro-1H-pyrazolo[3,4-b]pyridine-4-carboxylic acid ethyl ester (10 g, 44.3 mmol) and dioxane (400 ml). To this resulting suspension were added a saturated solution of sodium hydrogen carbonate (0.5M, 260 ml) and iodine (11.2 g, 44.3 mmol). The reaction mixture was stirred at room temperature for 24 hours, iodine was then added (25 g, 97.5 mmol) and stirring was pursued for 48 hours. Next an aqueous sodium thiosulfate solution (0.9M) was added until complete decolouration and was poured into a solution of ice and HCl at pH=2. The mixture was filtered to afford the title compound as a yellow solid (14.7 g, 95%).

後処理

  1. stirringstirring
  2. waitwas pursued for 48 hours
  3. filtrationThe mixture was filtered

出典と根拠

ORDレコード
ord-0feb0072c1d8407692aef2d36ab0e5e5
出典データセット
uspto-grants-2014_09
特許番号
US08846712B2

反応ノート

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