Potassium Carbonate → HCID 59860298、化合物

HRID 270705

反応式

HRID 270705 の反応式
[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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 2957694-Amino-2-(methylsulfanyl)pyrimidine-5-carbaldehydeHCID 23185255HCID 23185255、化合物

生成物 1

HCID 59860298HCID 59860298、化合物収率 80%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

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%).

後処理

  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%)

出典と根拠

ORDレコード
ord-e4f4a8f10e67450f8d1fa16affa1cd13
出典データセット
uspto-grants-2008_11
特許番号
US07449582B2

関連ノート

読み込み中…