Tetrahydrofuran → HCID 178473742、化合物

HRID 23161

反応式

HRID 23161 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([NH2:8])[CH2:4][CH2:3]1.Cl[C:10]1[N:11]([C:30](=[O:32])[CH3:31])[CH2:12][C:13]2[N:19]=[C:18]([Cl:20])[N:17]=[C:16]([NH:21][C:22]3[CH:27]=[CH:26][C:25]([F:28])=[C:24]([Cl:29])[CH:23]=3)[C:14]=2[N:15]=1.C1COCC1.C(N(CC)CC)C>O>[Cl:20][C:18]1[N:17]=[C:16]([NH:21][C:22]2[CH:27]=[CH:26][C:25]([F:28])=[C:24]([Cl:29])[CH:23]=2)[C:14]2[N:15]=[C:10]([NH:8][CH:5]3[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]3)[N:11]([C:30](=[O:32])[CH3:31])[CH2:12][C:13]=2[N:19]=1

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 27375314-Amino-1-methylpiperidineHCID 225929701-[2,6-Dichloro-8-(3-chloro-4-fluorophenylamino)-4H-pyrimido[5,4-d]pyrimidin-3-yl]ethanone

生成物 1

HCID 178473742HCID 178473742、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

47.2 g (0.413 mol) of 1-methyl-4-aminopiperidine is added dropwise at ambient temperature to a mixture of 123.3 g (0.317 mol) of (3), 740 ml of THF and 61.7 ml (0.445 mol) of triethylamine. The mixture is stirred for 30 min at 50° C. It is left to cool to 40° C., 1480 ml of water are added and the mixture is then stirred for 90 minutes at 10° C. The product that crystallises out is filtered off, washed with 150 ml of water and dried in vacuo at 60° C. The product is dissolved in 1150 ml of ethyl acetate at boiling temperature. It is cooled to 10° C., filtered and the product that crystallises out is dried at 60° C. in vacuo. Yield: 128.9 g (87.2%).

後処理

  1. waitIt is left
  2. temperatureto cool to 40° C.
  3. stirringthe mixture is then stirred for 90 minutes at 10° C
  4. customThe product that crystallises out
  5. filtrationis filtered off
  6. washwashed with 150 ml of water
  7. customdried in vacuo at 60° C
  8. dissolutionThe product is dissolved in 1150 ml of ethyl acetate
  9. temperatureIt is cooled to 10° C.
  10. filtrationfiltered
  11. customthe product that crystallises out
  12. customis dried at 60° C. in vacuo

出典と根拠

ORDレコード
ord-06a7203e45974abea770c02cd055dcd5
出典データセット
uspto-grants-2005_02
特許番号
US06849734B2

関連ノート

読み込み中…