Sodium Hydroxide → 3,4,5,6,7,8-Hexahydro-3-[2-(4-(2-methoxyphenyl)-1-piperazinyl)ethyl]pyrido[4',3'; 4,5]thieno[2,3-d]pyrimidin-4-one

HRID 1935465ノート

反応式

HRID 1935465 の反応式
C([N:4]1[CH2:33][CH2:32][C:7]2[C:8]3[C:13](=[O:14])[N:12]([CH2:15][CH2:16][N:17]4[CH2:22][CH2:21][N:20]([C:23]5[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=5[O:29][CH3:30])[CH2:19][CH2:18]4)[CH:11]=[N:10][C:9]=3[S:31][C:6]=2[CH2:5]1)(=O)C.[OH-].[Na+]>Cl>[CH3:30][O:29][C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=1[N:20]1[CH2:21][CH2:22][N:17]([CH2:16][CH2:15][N:12]2[C:13](=[O:14])[C:8]3[C:7]4[CH2:32][CH2:33][NH:4][CH2:5][C:6]=4[S:31][C:9]=3[N:10]=[CH:11]2)[CH2:18][CH2:19]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 98046243,4,5,6,7,8-Hexahydro-7-acetyl-3-[2-(4-(2-methoxyphenyl)-1-piperazinyl)ethyl]pyrido[4',3':4,5]thieno[2,3-d]pyrimidin-4-one

生成物 1

HCID 98886573,4,5,6,7,8-Hexahydro-3-[2-(4-(2-methoxyphenyl)-1-piperazinyl)ethyl]pyrido[4',3'; 4,5]thieno[2,3-d]pyrimidin-4-one収率 101.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
100 °C

実験手順

4.0 g (8.6 mmol) of 3,4,5,6,7,8-hexahydro-7-acetyl-3-[2-(4-(2-methoxyphenyl)piperazin-1-yl)ethyl]pyrido[4′,3′:4,5]thieno-[2,3-d]pyrimidin-4-one were dissolved in 80 ml of 10% strength hydrochloric acid and this solution was stirred at a bath temperature of 100° C. for 2 h. After that, the mixture was poured onto ice water and this mixture was rendered alkaline with conc. sodium hydroxide solution and extracted twice with methylene chloride. The combined organic phases were dried and evaporated. This resulted in the isolation of 3.7 g of crude product which was then recrystallized from 50 ml of isopropanol. 2.4 g (66%) of product having a m.p. of 168-170° C. were obtained.

後処理

  1. additionAfter that, the mixture was poured onto ice water
  2. extractionextracted twice with methylene chloride
  3. customThe combined organic phases were dried
  4. customevaporated

出典と根拠

ORDレコード
ord-d729167733764256bd2229a1f8d213eb
出典データセット
uspto-grants-2002_05
特許番号
US06387912B1

反応ノート

読み込み中…