Potassium Carbonate → HCID 59860298, 화합물

HRID 270705

반응식

HRID 270705 반응식
[NH2:1][C:2]1[C:7]([CH:8]=O)=[CH:6][N:5]=[C:4]([S:10][CH3:11])[N:3]=1.[NH2:12][C:13]1[C:14]([Cl:23])=[C:15]([CH2:20][C:21]#[N:22])[C:16]([Cl:19])=[CH:17][CH:18]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[NH2:12][C:13]1[C:14]([Cl:23])=[C:15]([C:20]2[C:21]([NH2:22])=[N:1][C:2]3[N:3]=[C:4]([S:10][CH3:11])[N:5]=[CH:6][C:7]=3[CH:8]=2)[C:16]([Cl:19])=[CH:17][CH:18]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2957694-Amino-2-(methylsulfanyl)pyrimidine-5-carbaldehydeHCID 23185255HCID 23185255, 화합물

생성물 1

HCID 59860298HCID 59860298, 화합물수율 80%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

A mixture of 4-amino-2-methylsulfanyl-pyrimidine-5-carbaldehyde (2.0 g, 11.82 mmol), (3-amino-2,6-dichloro-phenyl)-acetonitrile (2.85 g, 14.18 mmol) and K2CO3 (4.9 g, 35.49 mmol) in DMF (20 mL) is heated to 110° C. for 30 hours. The solution is cooled to room temperature and the solid is removed by filter paper and concentrated to give crude product. Flash silica gel column purification, eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/7%), gives the title intermediate as a solid (3.31 g, 80.0%).

후처리

  1. temperatureThe solution is cooled to room temperature
  2. customthe solid is removed
  3. filtrationby filter paper
  4. concentrationconcentrated
  5. customto give crude product
  6. customFlash silica gel column purification
  7. washeluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/7%)

출처 및 근거

ORD 기록
ord-e4f4a8f10e67450f8d1fa16affa1cd13
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449582B2

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