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

HRID 127273

反応式

HRID 127273 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a4e04b06a28b4d3a9bdb79429e524ff1
出典データセット
uspto-grants-1981_03
特許番号
US04255429

関連ノート

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