Toluene → 2-(4'-Benzyl-piperazino)-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidine

HRID 66002ノート

反応式

HRID 66002 の反応式
Cl[C:2]1[N:3]=[CH:4][C:5]2[C:11](=[O:12])[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:9][N:8]([CH2:18][CH3:19])[C:6]=2[N:7]=1.[CH2:20]([N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C1(C)C=CC=CC=1>C(Cl)(Cl)Cl.O>[CH2:20]([N:27]1[CH2:32][CH2:31][N:30]([C:2]2[N:3]=[CH:4][C:5]3[C:11](=[O:12])[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:9][N:8]([CH2:18][CH3:19])[C:6]=3[N:7]=2)[CH2:29][CH2:28]1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

参加物

6

反応物 3

HCID 1140TolueneHCID 759941-BenzylpiperazineHCID 122668052-Chloro-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydropyrido(2,3-d)pyrimidine

生成物 1

HCID 122668082-(4'-Benzyl-piperazino)-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidine収率 90%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

As described in Example VI, a mixture of 5.6 g. of 2-chloro-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydropyrido(2,3-d)pyrimidine, 7.04 g. of N-benzylpiperazine and 80 cm3 of toluene is heated under reflux for 2 hours. After cooling, the mass is diluted with 100 cm3 of chloroform and is taken up in 200 cm3 of water. After washing the organic phase with water, the reaction product is isolated as described in the Example mentioned. It is recrystallised from isopropanol. 7.6 g. (90%) of 2-(4'-benzyl-piperazino)-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidine are obtained; melting point 152° C.

後処理

  1. additiona mixture of 5.6 g
  2. temperatureunder reflux for 2 hours
  3. temperatureAfter cooling
  4. washAfter washing the organic phase with water
  5. customthe reaction product is isolated
  6. customIt is recrystallised from isopropanol

出典と根拠

ORDレコード
ord-fa47c2ad0e9e443182fecb169b01b9ea
出典データセット
uspto-grants-1978_12
特許番号
US04129737

反応ノート

読み込み中…