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Sodium Hydroxide → HCID 19083162、化合物

HRID 1378925
ノート
印刷プレビュー

反応式

HRID 1378925 の反応式
[NH2:1]OS(O)(=O)=O.[OH-].[Na+].[CH3:9][N:10]1[C:18]([S:19]([O-:21])=[O:20])=[C:17]2[C:12]([CH:13]=[CH:14][CH:15]=[CH:16]2)=[N:11]1.[Li+]>O>[CH3:9][N:10]1[C:18]([S:19]([NH2:1])(=[O:21])=[O:20])=[C:17]2[C:12]([CH:13]=[CH:14][CH:15]=[CH:16]2)=[N:11]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 76284hydroxylamine-O-sulfonic acidHCID 23675697HCID 23675697、化合物

生成物 1

HCID 19083162HCID 19083162、化合物収率 58%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
10 °C

実験手順

A solution containing 9.5 g (72 mmol) of 2-methyl-2H-indazole in 200 ml of ethyl ether, was cooled to -30° C., and 61.4 g (144 mmol) of n-butyl lithium (a 15% hexane solution) was dropwise added thereto. The mixture was stirred for one hour at the same temperature, and then an excess amount of sulfurous acid gas was blown thereinto for 3 hours at a temperature of not higher than -20° C. After completion of the reaction, the mixture was returned to room temperature, stirred for 12 hours and then diluted with ethyl ether. The product was subjected to filtration. The crystals were dried to obtain crude lithium 2-methyl-2H-indazole-3-sulfinate. This product was used for the subsequent reaction without purification. 48.8 g (430 mmol) of hydroxylamine-O-sulfonic acid was gradually added to a solution containing 17.2 g (430 mmol) of sodium hydroxide in water (300 ml) under cooling with ice (not higher than 10° C.). This solution was added all at once to a solution containing the crude lithium 2-methyl-2H-indazole-3-sulfinate previously prepared in water (100 ml), and then the mixture was stirred for 12 hours at room temperature. Formed crystals were collected by filtration to obtain 8.8 g (yield: 58%) of 2-methyl-2H-indazole-3-sulfonamide (slightly yellow granular crystals). Melting point: 181°-183° C.

後処理

  1. customThis product was used for the subsequent reaction without purification
  2. additionThis solution was added all at once to a solution
  3. customFormed crystals
  4. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-8c18e1f2b3f3425f998618d76aa06029
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05670452

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート