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

HRID 570021ノート

反応式

HRID 570021 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31260Isoamyl Alcohol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-30f053a88af04eaa9def24ea5c8be9d7
出典データセット
uspto-grants-1988_03
特許番号
US04734418

反応ノート

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