Tripropylamine → 6,7-Dimethoxy-2-(4-(5,6-dihydro-6-ethyl-5-oxopyrido[4,3-d]pyrimidine-2-yl)piperazino)quinazoline

HRID 570021노트

반응식

HRID 570021 반응식
C(N(CCC)CCC)CC.Cl[C:12]1[N:21]=[CH:20][C:19]2[C:14](=[CH:15][C:16]([O:24][CH3:25])=[C:17]([O:22][CH3:23])[CH:18]=2)[N:13]=1.[CH2:26]([N:28]1[CH:43]=[CH:42][C:31]2[N:32]=[C:33]([N:36]3[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]3)[N:34]=[CH:35][C:30]=2[C:29]1=[O:44])[CH3:27]>C(O)CC(C)C>[CH3:23][O:22][C:17]1[CH:18]=[C:19]2[C:14](=[CH:15][C:16]=1[O:24][CH3:25])[N:13]=[C:12]([N:39]1[CH2:38][CH2:37][N:36]([C:33]3[N:34]=[CH:35][C:30]4[C:29](=[O:44])[N:28]([CH2:26][CH3:27])[CH:43]=[CH:42][C:31]=4[N:32]=3)[CH2:41][CH2:40]1)[N:21]=[CH:20]2

참가 물질

5

반응물 3

HCID 7616TripropylamineHCID 18181442-Chloro-6,7-dimethoxyquinazolineHCID 137109456-ethyl-2-piperazinopyrido[4,3-d]pyrimidine-5(6H)-one

생성물 1

HCID 139212736,7-Dimethoxy-2-(4-(5,6-dihydro-6-ethyl-5-oxopyrido[4,3-d]pyrimidine-2-yl)piperazino)quinazoline수율 92.9%

시약·촉매·용매 1

HCID 31260Isoamyl Alcohol용매

실험 절차

Tri-n-propylamine (0.43 g) was added to 0.67 g of the 2-chloro-6,7-dimethoxyquinazoline synthesized in Referential Example 91 and 0.78 g of the 6-ethyl-2-piperazinopyrido[4,3-d]pyrimidine-5(6H)-one synthesized in Referential Example 14. Using 5 g of isoamyl alcohol as a solvent, they were heated and reacted for 10 hours under reflux. The resultant crystals were collected by filtration and then washed first with ethyl acetate and then with hexane. They were dried to obtain 1.24 g of the above-identified compound as white crystals (yield: 92%).

후처리

  1. customsynthesized in Referential Example 14
  2. temperaturethey were heated
  3. customreacted for 10 hours
  4. temperatureunder reflux
  5. filtrationThe resultant crystals were collected by filtration
  6. washwashed first with ethyl acetate
  7. customThey were dried

출처 및 근거

ORD 기록
ord-30f053a88af04eaa9def24ea5c8be9d7
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04734418

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