Sodium Iodide → 5-[1-(2-Bromo-phenylamino)-ethyl]-2-methylsulfanyl-pyrimidin-4-yl-methyl-amine

HRID 1247653ノート

反応式

HRID 1247653 の反応式
Cl[CH:2]([C:4]1[C:5]([NH:12][CH3:13])=[N:6][C:7]([S:10][CH3:11])=[N:8][CH:9]=1)[CH3:3].[I-].[Na+].[Br:16][C:17]1[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=1[NH2:19].C(N(C(C)C)C(C)C)C>C(#N)C.O>[Br:16][C:17]1[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=1[NH:19][CH:2]([C:4]1[C:5]([NH:12][CH3:13])=[N:6][C:7]([S:10][CH3:11])=[N:8][CH:9]=1)[CH3:3]

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 119922-BromoanilineHCID 81531DiisopropylethylamineHCID 21908981[5-(1-Chloro-ethyl)-2-methylsulfanyl-pyrimidin-4-yl]-methyl-amine

生成物 1

HCID 219089795-[1-(2-Bromo-phenylamino)-ethyl]-2-methylsulfanyl-pyrimidin-4-yl-methyl-amine収率 38.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒2 回

実験手順

0.25 g of the product from Example 11b, supra, and 34 mg sodium iodide in 10 mL acetonitrile were stirred for 15 min at RT. The resulting suspension was added drop-wise at RT to a mixture of 0.21 g 2-bromoaniline (Aldrich) and 0.33 g N-ethyl-di-isopropyl amine (Aldrich) in 5 mL acetonitrile. Stirring was continued for 16 hrs and the mixture was diluted with 20 mL water and extracted with dichloromethane. Chromatography on silica (eluent CHCl3) yielded 158 mg of the title product.

後処理

  1. additionThe resulting suspension was added drop-wise at RT
  2. extractionextracted with dichloromethane

出典と根拠

ORDレコード
ord-b4f91d0912544e099b5ce3690a144676
出典データセット
uspto-grants-2006_10
特許番号
US07129351B2

反応ノート

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