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

HRID 1768946

반응식

HRID 1768946 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
170 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ffaac1866e2e41fd8560fdae32cb8b29
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05380724

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