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

HRID 617177노트

반응식

HRID 617177 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5c90be30ff2f48d5968c44e2c79bb7f6
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05948786

반응 노트

불러오는 중…