Potassium Carbonate → 5,6-Dimethyl-3-amino-2-(2',5'-difluorobenzoyl)-thieno[2,3-b]pyridine

HRID 450856

反応式

HRID 450856 の反応式
C(=O)([O-])[O-].[K+].[K+].[F:7][C:8]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:9]=1[C:10](=[O:13])[CH2:11]Br.[CH3:19][C:20]1[C:21]([CH3:29])=[N:22][C:23]([SH:28])=[C:24]([CH:27]=1)[C:25]#[N:26]>CN(C=O)C.C(OCC)(=O)C>[CH3:19][C:20]1[CH:27]=[C:24]2[C:25]([NH2:26])=[C:11]([C:10](=[O:13])[C:9]3[CH:14]=[C:15]([F:18])[CH:16]=[CH:17][C:8]=3[F:7])[S:28][C:23]2=[N:22][C:21]=1[CH3:29]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 27782642-Bromo-1-(2,5-difluorophenyl)ethanoneHCID 178426634HCID 178426634、化合物

生成物 1

HCID 692802095,6-Dimethyl-3-amino-2-(2',5'-difluorobenzoyl)-thieno[2,3-b]pyridine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A suspension of potassium carbonate (0.399 g, 2.89 mmol), 2,5-difluorophenacyl bromide (0.408 g, 1.73 mmol) and 5,6-dimethyl-2-mercaptonicotine nitrile (0.19 g, 1.16 mmol) in dry DMF (4 ml) is stirred at room temperature for 16 h. The resulting mixture is diluted with ethyl acetate and washed with water. Drying over sodium sulfate, filtering, evaporating the solvent and purification of the residue by silicagel column chromatography yields the title compound with a m.p. of 188° C.

後処理

  1. washwashed with water
  2. dry with materialDrying over sodium sulfate
  3. filtrationfiltering
  4. customevaporating
  5. customthe solvent and purification of the residue by silicagel column chromatography

出典と根拠

ORDレコード
ord-4feec454f3c245e1b30ef272160fd095
出典データセット
uspto-grants-2013_07
特許番号
US08486996B2

関連ノート

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