Triethylamine → N-({4-[3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazol-1-yl]phenyl}methyl)-2-propanesulfonamide

HRID 1988687ノート

反応式

HRID 1988687 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[N:5]([C:12]2[CH:17]=[CH:16][C:15]([CH2:18][NH2:19])=[CH:14][CH:13]=2)[N:4]=1.C(N(CC)CC)C.[CH:29]([S:32](Cl)(=[O:34])=[O:33])([CH3:31])[CH3:30]>C(Cl)Cl>[F:21][C:2]([F:1])([F:20])[C:3]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[N:5]([C:12]2[CH:17]=[CH:16][C:15]([CH2:18][NH:19][S:32]([CH:29]([CH3:31])[CH3:30])(=[O:34])=[O:33])=[CH:14][CH:13]=2)[N:4]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 824082-Propanesulfonyl chlorideHCID 19627303({4-[3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazol-1-yl]phenyl}methyl)amine

生成物 1

HCID 24826368N-({4-[3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazol-1-yl]phenyl}methyl)-2-propanesulfonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of ({4-[3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazol-1-yl]phenyl}methyl)amine (100 mg, 0.339 mmol), triethylamine (0.07 ml, 0.51 mmol) in DCM (10 ml) was stirred in an ice bath under argon. Then isopropylsulfonyl chloride was added (148 mg in total, 1 mmol) in DCM (1 ml) dropwise with stirring. The reaction mixture was allowed to stir at room temperature for 16 hr. Then the reaction mixture was washed with water (20 ml), separated the organic layer and dried with sodium sulphate. Solvent was removed by rotary evaporation and the sample purified by MDAP to give the title compound as an off white solid (51 mg, 37%).

後処理

  1. stirringwith stirring
  2. stirringto stir at room temperature for 16 hr
  3. washThen the reaction mixture was washed with water (20 ml)
  4. customseparated the organic layer
  5. dry with materialdried with sodium sulphate
  6. customSolvent was removed by rotary evaporation
  7. customthe sample purified by MDAP

出典と根拠

ORDレコード
ord-eed80257052547daa3730ddcb637f6be
出典データセット
uspto-grants-2010_01
特許番号
US07642256B2

反応ノート

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