1-Methyl-3-(trifluoroacetyl)-1H-indole → HCID 59437267、化合物

HRID 244463

反応式

HRID 244463 の反応式
Br[C:2]1[CH:18]=[CH:17][C:5]2[N:6]([C:10]3[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=3)[C:7](=[O:9])[NH:8][C:4]=2[CH:3]=1.C([Li])CCC.[F:24][C:25]([F:39])([F:38])[C:26]([C:28]1[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[N:30]([CH3:37])[CH:29]=1)=[O:27]>COCCOCCOC.CCOCC>[F:16][C:13]1[CH:14]=[CH:15][C:10]([N:6]2[C:5]3[CH:17]=[CH:18][C:2]([C:26]([OH:27])([C:28]4[C:36]5[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=5)[N:30]([CH3:37])[CH:29]=4)[C:25]([F:24])([F:39])[F:38])=[CH:3][C:4]=3[NH:8][C:7]2=[O:9])=[CH:11][CH:12]=1

参加物

6

反応物 3

HCID 35243881-Methyl-3-(trifluoroacetyl)-1H-indoleHCID 59437201HCID 59437201、化合物HCID 178418339Butyllithium

生成物 1

HCID 59437267HCID 59437267、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8150Diglyme溶媒

実験手順

To a chilled (−78° C.) solution of 5-bromo-1-(4-fluorophenyl)-1,3-dihydrobenzimidazol-2-one (152 mg, 0.5 mmol) in anhydrous bis(2-methoxyethyl)ether (10 mL) was added 0.5 mL (1.25 mmol) of a solution of 2.5 M n-butyllithium in hexanes. After 30 minutes, a solution of 2,2,2-trifluoro-1-(1-methyl-1H-indol-3-yl)ethanone (114 mg) in bis(2-methoxyethyl) in 1 mL of ether was added. The mixture stirred for 1 hour and was quenched with ammonium chloride solution. The resulting precipitate was filtered, washed with water, and dried to afford the title compound as an off-white solid. MS m/z 456 (MH+).

後処理

  1. customwas quenched with ammonium chloride solution
  2. filtrationThe resulting precipitate was filtered
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-6fd87ebebfdd4b239aa9588f5450b660
出典データセット
uspto-grants-2014_02
特許番号
US08658637B2

関連ノート

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