Methane → 6-(4-Amino-4-methylpiperidin-1-yl)-4-(3-chloro-4-fluorophenylamino)-pyrimido[5,4-d]pyrimidine

HRID 23163

反応式

HRID 23163 の反応式
[NH2:1][C:2]1([CH3:28])[CH2:7][CH2:6][N:5]([C:8]2[NH:9][CH2:10][C:11]3[N:12]=[C:13](Cl)[N:14]=[C:15]([NH:18][C:19]4[CH:24]=[CH:23][C:22]([F:25])=[C:21]([Cl:26])[CH:20]=4)[C:16]=3[N:17]=2)[CH2:4][CH2:3]1.I.C>C(O)(=O)C>[NH2:1][C:2]1([CH3:28])[CH2:3][CH2:4][N:5]([C:8]2[N:9]=[CH:10][C:11]3[N:12]=[CH:13][N:14]=[C:15]([NH:18][C:19]4[CH:24]=[CH:23][C:22]([F:25])=[C:21]([Cl:26])[CH:20]=4)[C:16]=3[N:17]=2)[CH2:6][CH2:7]1

参加物

5

反応物 3

HCID 297MethaneHCID 24841Hydrogen iodideHCID 178432946HCID 178432946、化合物

生成物 1

HCID 99522166-(4-Amino-4-methylpiperidin-1-yl)-4-(3-chloro-4-fluorophenylamino)-pyrimido[5,4-d]pyrimidine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
15 °C

実験手順

A mixture of 80 g (0.182 mol) of (6) in 160 ml glacial acetic acid at 90° C. is added dropwise to a suspension of 11.7 g (0.378 mol) of red phosphorus in 150 ml of hydriodic acid (57%, 1.134 mol). The mixture is refluxed for 4 hours, 5 g of activated charcoal are added, the mixture is then filtered and the residue is washed with glacial acetic acid and water. The filtrate is added dropwise, with vigorous stirring, to a solution of 270 ml water, 270 ml of methanol and 270 ml of sodium hydroxide solution (50%). The mixture is stirred for a further 30 minutes at 15° C. and the solid precipitated is filtered off. This is washed twice with 500 ml of water, then suspended in 500 ml of water, filtered off and dried in vacuo at 45° C. Yield: 65.2 g (91.9%)

後処理

  1. temperatureThe mixture is refluxed for 4 hours
  2. filtrationthe mixture is then filtered
  3. washthe residue is washed with glacial acetic acid and water
  4. additionThe filtrate is added dropwise, with vigorous stirring, to a solution of 270 ml water, 270 ml of methanol and 270 ml of sodium hydroxide solution (50%)
  5. customthe solid precipitated
  6. filtrationis filtered off
  7. washThis is washed twice with 500 ml of water
  8. filtrationfiltered off
  9. customdried in vacuo at 45° C

出典と根拠

ORDレコード
ord-08dad2180b5a4c7daee879baeb9b8b5e
出典データセット
uspto-grants-2005_02
特許番号
US06849734B2

関連ノート

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