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 1935465노트

반응식

HRID 1935465 반응식
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

참가 물질

4

반응물 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

생성물 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-one수율 101.1%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d729167733764256bd2229a1f8d213eb
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06387912B1

반응 노트

불러오는 중…