Sodium hydride → HCID 68159499、化合物

HRID 508196ノート

反応式

HRID 508196 の反応式
[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

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 27362353,5-Dimethylbenzenesulfonyl chlorideHCID 178419483HCID 178419483、化合物

生成物 1

HCID 68159499HCID 68159499、化合物収率 38.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e24a3adcca4a4e009f99988e51e84bb3
出典データセット
uspto-grants-2015_08
特許番号
US09095583B2

反応ノート

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