Trimethylsilyl isocyanate → [4-(4-Chloro-5-methylsulfanyl-6-morpholin-4-yl-pyrimidin-2-yl)-phenyl]-urea

HRID 629010ノート

反応式

HRID 629010 の反応式
C[Si]([N:5]=[C:6]=[O:7])(C)C.[Cl:8][C:9]1[C:14]([S:15][CH3:16])=[C:13]([N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[N:12]=[C:11]([C:23]2[CH:28]=[CH:27][C:26]([NH2:29])=[CH:25][CH:24]=2)[N:10]=1>C1COCC1>[Cl:8][C:9]1[C:14]([S:15][CH3:16])=[C:13]([N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[N:12]=[C:11]([C:23]2[CH:28]=[CH:27][C:26]([NH:29][C:6]([NH2:5])=[O:7])=[CH:25][CH:24]=2)[N:10]=1

参加物

4

反応物 2

HCID 70696Trimethylsilyl isocyanateHCID 86673495HCID 86673495、化合物

生成物 1

HCID 86673497[4-(4-Chloro-5-methylsulfanyl-6-morpholin-4-yl-pyrimidin-2-yl)-phenyl]-urea収率 31.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Trimethylsilyl isocyanate (136 mg, 5 eq.) was added to a stirred solution of 4-(4-Chloro-5-methylsulfanyl-6-morpholin-4-yl-pyrimidin-2-yl)-phenylamine (80 mg, 0.237 mmol.) in THF (2.0 ml) and the mixture was reacted to reflux for 16 hrs. The reaction mixture was extracted with EA and washed with brine. The crude was purified by Chromatography (Hexane/EtOAc 1:1) to give a product 28.1 mg (31.2%).

後処理

  1. customthe mixture was reacted
  2. temperatureto reflux for 16 hrs
  3. extractionThe reaction mixture was extracted with EA
  4. washwashed with brine
  5. customThe crude was purified by Chromatography (Hexane/EtOAc 1:1)

出典と根拠

ORDレコード
ord-8f3dca6440bc480696c3a6da501d985f
出典データセット
uspto-grants-2016_04
特許番号
US09315491B2

反応ノート

読み込み中…