Sodium hydride → HCID 68159499, 화합물

HRID 508196

반응식

HRID 508196 반응식
[Br:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:4][N:3]=1.[H-].[Na+].[CH3:13][C:14]1[CH:15]=[C:16]([S:21](Cl)(=[O:23])=[O:22])[CH:17]=[C:18]([CH3:20])[CH:19]=1>CN(C=O)C>[Br:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([S:21]([C:16]2[CH:17]=[C:18]([CH3:20])[CH:19]=[C:14]([CH3:13])[CH:15]=2)(=[O:23])=[O:22])[N:3]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 27362353,5-Dimethylbenzenesulfonyl chlorideHCID 178419483HCID 178419483, 화합물

생성물 1

HCID 68159499HCID 68159499, 화합물수율 38.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3-bromo-1H-indazole (3 gram; 15 mmol) was dissolved in 30 ml DMF, followed by the addition of sodiumhydride (850 mg, 21 mmol). After stirring for 20 min at room temperature, 3,5-dimethylbenzene-1-sulfonyl chloride (4.4 gram, 21 mmol) was added and the reaction mixture was stirred for another 2 h at room temperature. The reaction was quenched by the addition of water and the formed solids were filtered off and washed with little methanol. The solids were dried to obtain 3-bromo-1-(3,5-dimethylphenylsulfonyl)-1H-indazole (2.1 gram) as a white solid.

후처리

  1. stirringthe reaction mixture was stirred for another 2 h at room temperature
  2. customThe reaction was quenched by the addition of water
  3. filtrationthe formed solids were filtered off
  4. washwashed with little methanol
  5. customThe solids were dried

출처 및 근거

ORD 기록
ord-e24a3adcca4a4e009f99988e51e84bb3
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09095583B2

연결된 노트

불러오는 중…