Sodium Hydroxide → 4-(1-Acetyl-4-piperidinyl)-2-aminoquinazoline

HRID 617177ノート

反応式

HRID 617177 の反応式
[NH2:1][C:2]1[N:11]=[C:10]([CH:12]2[CH2:17][CH2:16][N:15]([C:18](=[O:25])[C:19]3C=CC=CC=3)[CH2:14][CH2:13]2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[OH-].[Na+]>C(O)C>[C:18]([N:15]1[CH2:16][CH2:17][CH:12]([C:10]2[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=[C:2]([NH2:1])[N:11]=2)[CH2:13][CH2:14]1)(=[O:25])[CH3:19]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 154287732-Amino-4-(1-benzoyl-4-piperidinyl)quinazoline

生成物 1

HCID 154287764-(1-Acetyl-4-piperidinyl)-2-aminoquinazoline収率 66.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-amino-4-(1-benzoyl-4-piperidinyl)quinazoline (24 g, 0.072 mol) obtained in Example 8 (3), ethanol (250 ml) and 6N sodium hydroxide aqueous solution (250 ml) was refluxed for about 7 hours under a nitrogen atmosphere. Thereafter ethanol was removed from the reaction mixture in vacuo. The residue was extracted with dichloromethane. The organic layer was washed with saturated sodium chloride aqueous solution, and then dried over magnesium sulfate and evaporated in vacuo. The residue was crystallized from isopropyl alcohol to give 13.0 g of the titled compound.

後処理

  1. temperaturewas refluxed for about 7 hours under a nitrogen atmosphere
  2. customThereafter ethanol was removed from the reaction mixture in vacuo
  3. extractionThe residue was extracted with dichloromethane
  4. washThe organic layer was washed with saturated sodium chloride aqueous solution
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was crystallized from isopropyl alcohol

出典と根拠

ORDレコード
ord-5c90be30ff2f48d5968c44e2c79bb7f6
出典データセット
uspto-grants-1999_09
特許番号
US05948786

反応ノート

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