Potassium Carbonate → 4-[(5-Cyano-2-methylsulfanyl-pyrimidin-4-ylamino)-methyl]-benzoic acid methyl ester

HRID 852943

반응식

HRID 852943 반응식
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][N:5]=[C:4]([S:10][CH3:11])[N:3]=1.[CH3:12][O:13][C:14](=[O:23])[C:15]1[CH:20]=[CH:19][C:18]([CH2:21]Br)=[CH:17][CH:16]=1.C([O-])([O-])=O.[K+].[K+]>COCCOC>[CH3:12][O:13][C:14](=[O:23])[C:15]1[CH:20]=[CH:19][C:18]([CH2:21][NH:1][C:2]2[C:7]([C:8]#[N:9])=[CH:6][N:5]=[C:4]([S:10][CH3:11])[N:3]=2)=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 256687Methyl 4-(bromomethyl)benzoateHCID 2957574-Amino-2-(methylsulfanyl)pyrimidine-5-carbonitrile

생성물 1

HCID 666222874-[(5-Cyano-2-methylsulfanyl-pyrimidin-4-ylamino)-methyl]-benzoic acid methyl ester

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
60 °C

실험 절차

To a solution of 4-amino-2-methylsulfanyl-pyrimidine-5-carbonitrile (229a) (200 mg, 1.2 mmol) in DME (10 ml) were added 4-bromomethyl-benzoic acid methyl ester (274 mg, 1.2 mmol) and K2CO3 (663 mg, 4.8 mmol) at room temperature. The reaction mixture was heated at 100° C. for 5 h, overnight at 60° C., cooled, filtered and concentrated in vacuo. The crude product was used in the next reaction without further purification. LRMS: 314.3(calc.); 315.3 (obt.) (MH)+.

후처리

  1. temperaturecooled
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. customThe crude product was used in the next reaction without further purification

출처 및 근거

ORD 기록
ord-305f829a2be54efc9c66e8294b34d4a4
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253204B2

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