Dimethyl Sulfoxide → HCID 67097502, 화합물

HRID 2077081노트

반응식

HRID 2077081 반응식
Cl[C:2]1[N:9]=[C:8]([NH:10][C:11]2[CH:15]=[C:14]([CH3:16])[NH:13][N:12]=2)[CH:7]=[C:6]([CH3:17])[C:3]=1[C:4]#[N:5].Cl.[F:19][C:20]1[CH:29]=[CH:28][C:23]([O:24][CH2:25][CH2:26][NH2:27])=[CH:22][CH:21]=1.C(=O)([O-])O.[Na+].CS(C)=O>O>[F:19][C:20]1[CH:29]=[CH:28][C:23]([O:24][CH2:25][CH2:26][NH:27][C:2]2[N:9]=[C:8]([NH:10][C:11]3[CH:15]=[C:14]([CH3:16])[NH:13][N:12]=3)[CH:7]=[C:6]([CH3:17])[C:3]=2[C:4]#[N:5])=[CH:22][CH:21]=1

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 516892Sodium BicarbonateHCID 11983545HCID 11983545, 화합물HCID 22061356Ethanamine, 2-(4-fluorophenoxy)-, hydrochloride (1:1)

생성물 1

HCID 67097502HCID 67097502, 화합물수율 4.3%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

Compound A (200 mg, 813 mmol), 2-(4-fluorophenoxy)ethylamine hydrochloride (466 mg) and sodium hydrogencarbonate (683 mg) were added to DMSO (6 ml), and the mixture was stirred at 100° C. for 27 hr. After stirring, the reaction mixture was added to cold water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and concentrated, and the residue was washed by suspending in ethyl acetate to give the object compound of 2-(2-(4-fluorophenoxy)ethylamino)-6-(5-methyl-1H-pyrazol-3-ylamino)-4-methylnicotinonitrile (38 mg).

후처리

  1. stirringAfter stirring
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. concentrationconcentrated
  5. washthe residue was washed

출처 및 근거

ORD 기록
ord-5520bf7e97f147e0a90cfa05412c23bf
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07928126B2

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