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

HRID 450856

반응식

HRID 450856 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4feec454f3c245e1b30ef272160fd095
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486996B2

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