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

HRID 2260561

反応式

HRID 2260561 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 18998616N-benzyloxycarbonyl-4,6-diaminopyrimidine収率 36.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-c1a138af9c1841a4a3c5349e166eb593
出典データセット
uspto-grants-1995_12
特許番号
US05478838

関連ノート

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