Potassium Carbonate → HCID 18446520、化合物

HRID 1268834ノート

反応式

HRID 1268834 の反応式
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][NH2:8])=[CH:5][CH:4]=1.C([O-])([O-])=O.[K+].[K+].[Br:17][C:18]1[S:26][C:25]2[C:24]([C:27]#[N:28])=[CH:23][N:22]=[C:21](Cl)[C:20]=2[CH:19]=1>CN1CCCC1=O>[Br:17][C:18]1[S:26][C:25]2[C:24]([C:27]#[N:28])=[CH:23][N:22]=[C:21]([NH:8][CH2:7][C:6]3[CH:9]=[CH:10][C:3]([O:2][CH3:1])=[CH:4][CH:5]=3)[C:20]=2[CH:19]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 754524-MethoxybenzylamineHCID 184465172-Bromo-4-chlorothieno[3,2-c]pyridine-7-carbonitrile

生成物 1

HCID 18446520HCID 18446520、化合物収率 66.5%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
130 °C

実験手順

To a stirred solution of 4-methoxybenzylamine (1.2 equiv., 2.4 mmol) and K2CO3 (2.4 equiv., 4.8 mmol) in 5 mL anhydrous 1-methyl-2-pyrrolidinone was added 15 (1 equiv., 2 mmol). The mixture was heated at 130° C. under N2 for 1.5 h, allowed to cool, and the product precipitated by the addition of H2O (5 mL). The mixture was filtered, washed with water, and dried, yielding 16 (1.33 mmol) as a brown solid. 1H NMR (400 MHz, d6-DMSO) δ: 8.75 (1H, t, broad), 8.56 (1H, s), 8.21 (1H, s), 7.43 (2H, d, J=8.6 Hz), 7.04 (2H, d, J=8.6), 4.84 (2H, d, J=5.8), 3.88 (3H, s).

後処理

  1. temperatureto cool
  2. customthe product precipitated by the addition of H2O (5 mL)
  3. filtrationThe mixture was filtered
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-9aeb3376fc80455a9d00abaf6cac3211
出典データセット
uspto-grants-2007_04
特許番号
US07199119B2

反応ノート

読み込み中…