Triethylamine → 2-[4-(3,4-Methylenedioxycinnamoyl)-piperazin-1-yl]-4-amino-6,7-dimethoxyquinazoline

HRID 1449160ノート

反応式

HRID 1449160 の反応式
[CH2:1]1[O:14][C:13]2[CH:12]=[CH:11][C:5]([CH:6]=[CH:7][C:8]([OH:10])=O)=[CH:4][C:3]=2[O:2]1.C(N(CC)CC)C.C(Cl)(=O)OCC.Cl.[N:29]1([C:35]2[N:44]=[C:43]([NH2:45])[C:42]3[C:37](=[CH:38][C:39]([O:48][CH3:49])=[C:40]([O:46][CH3:47])[CH:41]=3)[N:36]=2)[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1>O.C(OCC)(=O)C>[CH2:1]1[O:14][C:13]2[CH:12]=[CH:11][C:5]([CH:6]=[CH:7][C:8]([N:32]3[CH2:33][CH2:34][N:29]([C:35]4[N:44]=[C:43]([NH2:45])[C:42]5[C:37](=[CH:38][C:39]([O:48][CH3:49])=[C:40]([O:46][CH3:47])[CH:41]=5)[N:36]=4)[CH2:30][CH2:31]3)=[O:10])=[CH:4][C:3]=2[O:2]1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 169173-(1,3-Benzodioxol-5-yl)prop-2-enoic acidHCID 204738332-Piperazine-4-amino-6,7-dimethoxy quinoline hydrochloride

生成物 1

HCID 537467432-[4-(3,4-Methylenedioxycinnamoyl)-piperazin-1-yl]-4-amino-6,7-dimethoxyquinazoline

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 346 mg. of 3,4-methylenedioxycinnamic acid and 364 mg. of triethylamine in 20 ml. of ethyl acetate were added under ice-cooling 195 mg. of ethyl chlorocarbonate and the resulting mixture was then stirred for 4 hours. Then, 543 mg. of 2-(piperazin-1-yl)-4-amino-6,7-dimethoxyquinazoline.hydrochloride were added thereto and the resulting mixture was stirred at room temperature overnight. After 50 ml. of water were added, the precipitate thus separated was recovered by filtration. The resulting crystalline substance was recrystallized from ethanol to give 320 mg. of the desired product as the hydrochloride.

後処理

  1. temperaturecooling 195 mg
  2. customthe precipitate thus separated
  3. filtrationwas recovered by filtration
  4. customThe resulting crystalline substance was recrystallized from ethanol
  5. customto give 320 mg

出典と根拠

ORDレコード
ord-6527e5e8b3a54e1faca099a64fd1412d
出典データセット
uspto-grants-1980_02
特許番号
US04189484

反応ノート

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