Sulfurous Acid → HCID 23675696、化合物

HRID 1378935ノート

反応式

HRID 1378935 の反応式
[Cl:1][C:2]1[C:3]2[C:7]([CH:8]=[CH:9][CH:10]=1)=[N:6][N:5]([CH3:11])[CH:4]=2.C([Li:16])CCC.[S:17](=O)([OH:19])[OH:18]>C(OCC)C>[Cl:1][C:2]1[C:3]2[C:7]([CH:8]=[CH:9][CH:10]=1)=[N:6][N:5]([CH3:11])[C:4]=2[S:17]([O-:19])=[O:18].[Li+:16]

参加物

5

反応物 3

HCID 1100Sulfurous AcidHCID 190831754-Chloro-2-methyl-2H-indazoleHCID 178418339Butyllithium

生成物 1

HCID 23675696HCID 23675696、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
-30 °C

実験手順

A solution containing 16 g (0.1 mol) of 4-chloro-2-methyl-2H-indazole in 300 ml of ethyl ether, was cooled to -30° C., and 85.4 g (0.2 mol) of n-butyl lithium (15% hexane solution) was dropwise added thereto. The mixture was stirred for one hour at the same temperature. Then, an excess amount of sulfurous acid gas was blown thereinto at a temperature of not higher than -20° C. for 3 hours. After completion of the reaction, the mixture was returned to room temperature and diluted with ethyl ether, and the product was subjected to filtration. Crystals were dried to obtain crude lithium 4-chloro-2-methyl-2H-indazole-3-sulfinate. This product was used for the subsequent reaction without purification.

後処理

  1. waitat a temperature of not higher than -20° C. for 3 hours
  2. customAfter completion of the reaction
  3. customwas returned to room temperature
  4. filtrationthe product was subjected to filtration
  5. customCrystals were dried

出典と根拠

ORDレコード
ord-99b3e4c3adbb4f988bae7c1bd2c23ce4
出典データセット
uspto-grants-1997_09
特許番号
US05670452

反応ノート

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