Hydrochloric Acid → 2,4-Diallylamino-6-aminoquinazoline

HRID 1250566ノート

反応式

HRID 1250566 の反応式
O.O.[Sn](Cl)Cl.Cl.[CH2:7]([NH:10][C:11]1[N:20]=[C:19]([NH:21][CH2:22][CH:23]=[CH2:24])[C:18]2[C:13](=[CH:14][CH:15]=[C:16]([N+:25]([O-])=O)[CH:17]=2)[N:12]=1)[CH:8]=[CH2:9].[OH-].[Na+]>>[CH2:7]([NH:10][C:11]1[N:20]=[C:19]([NH:21][CH2:22][CH:23]=[CH2:24])[C:18]2[C:13](=[CH:14][CH:15]=[C:16]([NH2:25])[CH:17]=2)[N:12]=1)[CH:8]=[CH2:9]

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 61436Stannous chloride dihydrateHCID 571174462,4-Diallylamino-6-nitroquinazoline

生成物 1

HCID 207186892,4-Diallylamino-6-aminoquinazoline

実験手順

To 3.32 g (14.73 mmol) of tin (II) chloride dihydrate was added 14 ml of concentrated hydrochloric acid and 1.40 g (4.91 mmol) of 2,4-diallylamino-6-nitroquinazoline under ice cooling, and the resulting mixture was stirred at room temperature overnight. The reaction mixture was neutralized by adding an aqueous sodium hydroxide solution, followed by extraction with chloroform, washing with brine and drying over anhydrous sodium sulfate. After the solvent was distilled off, the residue was purified by a silica gel column to give 1.61 g (yield: 92.5%) of a free base compound of the title compound.

後処理

  1. extractionfollowed by extraction with chloroform
  2. washwashing with brine
  3. dry with materialdrying over anhydrous sodium sulfate
  4. distillationAfter the solvent was distilled off
  5. customthe residue was purified by a silica gel column

出典と根拠

ORDレコード
ord-1c114146388443129996fd05d61419bc
出典データセット
uspto-grants-2002_01
特許番号
US06339089B2

反応ノート

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