Sodium Carbonate → 1-[1-(4-Amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-4,4-dimethyl-piperidin-2,6-dione monohydrochloride

HRID 127273

반응식

HRID 127273 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([Cl:16])[N:3]=1.[CH3:17][C:18]1([CH3:32])[CH2:23][C:22](=[O:24])[N:21]([CH:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)[C:20](=[O:31])[CH2:19]1.C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O>[ClH:16].[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:28]2[CH2:29][CH2:30][CH:25]([N:21]3[C:20](=[O:31])[CH2:19][C:18]([CH3:17])([CH3:32])[CH2:23][C:22]3=[O:24])[CH2:26][CH2:27]2)[N:3]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 902352-Chloro-6,7-dimethoxy-4-quinazolinamineHCID 128225624,4-Dimethyl[1,4'-bipiperidine]-2,6-dione

생성물 1

HCID 205562601-[1-(4-Amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-4,4-dimethyl-piperidin-2,6-dione monohydrochloride

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

The mixture of 4.79 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline, 4.49 g of 4,4-dimethyl-1-(4-piperidinyl)-piperidin-2,6-dione, 4.24 g of anhydrous sodium carbonate and 75 ml of dimethylformamide is stirred at 150° under nitrogen for 6 hours. It is filtered, the filtrate evaporated, the residue dissolved in ethyl acetate and the solution washed with aqueous sodium carbonate and water. It is dried, evaporated, the residue triturated with isopropanol, filtered off and discarded. The filtrate is made strongly acidic with hydrogen chloride, the precipitate filtered off and triturated with 175 ml of boiling methanol, to yield the 1-[1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-4,4-dimethyl-piperidin-2,6-dione monohydrochloride, melting at 279°-280° with decomposition.

후처리

  1. filtrationIt is filtered
  2. customthe filtrate evaporated
  3. dissolutionthe residue dissolved in ethyl acetate
  4. washthe solution washed with aqueous sodium carbonate and water
  5. customIt is dried
  6. customevaporated
  7. customthe residue triturated with isopropanol
  8. filtrationfiltered off
  9. filtrationthe precipitate filtered off
  10. customtriturated with 175 ml of boiling methanol

출처 및 근거

ORD 기록
ord-a4e04b06a28b4d3a9bdb79429e524ff1
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255429

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