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

HRID 1449160노트

반응식

HRID 1449160 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6527e5e8b3a54e1faca099a64fd1412d
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04189484

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