Piperazine, 1-(1-adamantyl)- → 1-(1-Adamantyl)-4-(2,6-diamino-4-pyrimidinyl)-piperazine

HRID 1768946

反応式

HRID 1768946 の反応式
[NH2:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4]([NH2:9])[N:3]=1.[C:10]12([N:20]3[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]3)[CH2:19][CH:14]3[CH2:15][CH:16]([CH2:18][CH:12]([CH2:13]3)[CH2:11]1)[CH2:17]2>C(O)C>[C:10]12([N:20]3[CH2:25][CH2:24][N:23]([C:6]4[CH:5]=[C:4]([NH2:9])[N:3]=[C:2]([NH2:1])[N:7]=4)[CH2:22][CH2:21]3)[CH2:17][CH:16]3[CH2:15][CH:14]([CH2:13][CH:12]([CH2:18]3)[CH2:11]1)[CH2:19]2

参加物

4

反応物 2

HCID 35373Piperazine, 1-(1-adamantyl)-HCID 674322,4-Diamino-6-chloropyrimidine

生成物 1

HCID 189463001-(1-Adamantyl)-4-(2,6-diamino-4-pyrimidinyl)-piperazine収率 80.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
170 °C

実験手順

A mixture of 2,6-diamino-4-chloropyrimidine (0.43 g, 3.0 mmol) and 1-(1-adamantyl)-piperazine (0.66 g, 3.0 mmol) in ethanol (30 ml) was heated in a sealed tube at 170° C. for 3 hours. After cooling the solvent was removed, the solid residue was dissolved in water (45 ml) and acidified to pH=3 with conc. HCl. The obtained mixture was heated to 50° C. the insolubles were filtered off and the clear solution was rendered alkaline with 10N NaOH under stirring and cooling. The precipitated crystals were collected, washed with water until neutral and dried. In this manner 0.79 g of the title compound was obtained in the form of its monohydrate, yield: 76.6%, mp. 265°-268° C.

後処理

  1. temperatureAfter cooling the solvent
  2. customwas removed
  3. dissolutionthe solid residue was dissolved in water (45 ml)
  4. temperatureThe obtained mixture was heated to 50° C. the insolubles
  5. filtrationwere filtered off
  6. temperaturecooling
  7. customThe precipitated crystals were collected
  8. washwashed with water until neutral and
  9. customdried

出典と根拠

ORDレコード
ord-ffaac1866e2e41fd8560fdae32cb8b29
出典データセット
uspto-grants-1995_01
特許番号
US05380724

関連ノート

読み込み中…