Hydrochloric Acid → N-benzyloxycarbonyl-4,6-diaminopyrimidine

HRID 2260561

반응식

HRID 2260561 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([NH2:8])[N:5]=[CH:4][N:3]=1.[OH-].[Na+].Cl.[CH2:12]([O:19][C:20](Cl)=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>O.C(O)C>[CH2:12]([O:19][C:20]([N:3]1[C:2]([NH2:1])=[CH:7][C:6]([NH2:8])=[N:5][CH2:4]1)=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10387Benzyl chloroformateHCID 14798Sodium HydroxideHCID 79608Pyrimidine-4,6-diamine

생성물 1

HCID 18998616N-benzyloxycarbonyl-4,6-diaminopyrimidine수율 36.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a mixture of 4,6-diaminopyrimidine (4.7 g), ethanol (500 ml) and water (200 ml) was added 1N sodium hydroxide (13.25 ml) while cooling with ice water. After the dropwise addition of 1N hydrochloric acid (26.5 ml) thereto, benzyloxycarbonyl chloride (4.5 g) was dropwise added thereto. After being stirred at room temperature for 2 hours, the mixture was concentrated under reduced pressure to give crystals. The crystals were collected by filtration and recrystallized from chloroform:methanol=5:1 to give 2.4 g of N-benzyloxycarbonyl-4,6-diaminopyrimidine, melting point 194° C.

후처리

  1. concentrationthe mixture was concentrated under reduced pressure
  2. customto give crystals
  3. filtrationThe crystals were collected by filtration
  4. customrecrystallized from chloroform

출처 및 근거

ORD 기록
ord-c1a138af9c1841a4a3c5349e166eb593
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05478838

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