Pentylamine → N-(2-Amino-5-benzyl-6-methylpyrimidine-4-yl)-N-pentylamine

HRID 965664

反応式

HRID 965664 の反応式
[CH2:1]([C:8]1[C:9](Cl)=[N:10][C:11]([NH2:15])=[N:12][C:13]=1[CH3:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:17]([NH2:22])[CH2:18][CH2:19][CH2:20][CH3:21]>O1CCOCC1>[NH2:15][C:11]1[N:10]=[C:9]([NH:22][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[C:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[C:13]([CH3:14])[N:12]=1

参加物

4

反応物 2

HCID 8060PentylamineHCID 8202385-Benzyl-4-chloro-6-methylpyrimidin-2-amine

生成物 1

HCID 12043763N-(2-Amino-5-benzyl-6-methylpyrimidine-4-yl)-N-pentylamine収率 89.7%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 5-benzyl-4-chloro-6-methylpyrimidine-2-ylamine (500 mg, 2.14 mmol), amylamine (1.24 ml) and dioxane (4 ml) was kept at 95-100° C. for 19 hours. The reaction mixture was concentrated in vacuo, and the residue was extracted with chloroform and a saturated aqueous NaHCO3 solution. The organic layer was washed with saturated brine, dried over sodium sulfate, and concentrated in vacuo. The residue was purified by silica gel column chromatography (2% MeOH/CHCl3) to give the object compound (546 mg, 89.7%).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. extractionthe residue was extracted with chloroform
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by silica gel column chromatography (2% MeOH/CHCl3)

出典と根拠

ORDレコード
ord-9f103579a5974a6dbb5baa6adf201994
出典データセット
uspto-grants-2005_10
特許番号
US06951866B2

関連ノート

読み込み中…