Sulfurous Acid → HCID 23675696, 화합물

HRID 963670노트

반응식

HRID 963670 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 23675696HCID 23675696, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
-30 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cbfb110301744a1d85082f57aa47c643
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763616

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