1,2-Dichloroethane → 6-(4-Chlorobenzyl)-1-(2,4-dichlorobenzenesulfonyl)-8-isopropyl-3-pyrrol-1-ylhexahydropyrazino[1,2-a]pyrimidine-4,7-dione

HRID 1994398노트

반응식

HRID 1994398 반응식
Br.[Cl:2][C:3]1[CH:36]=[CH:35][C:6]([CH2:7][CH:8]2[N:13]3[C:14](=[O:30])[CH:15]([NH2:29])[CH2:16][N:17]([S:18]([C:21]4[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=4[Cl:28])(=[O:20])=[O:19])[CH:12]3[CH2:11][N:10]([CH:31]([CH3:33])[CH3:32])[C:9]2=[O:34])=[CH:5][CH:4]=1.ClCCCl.CO[CH:43]1[CH2:47][CH2:46][CH:45](OC)O1>O>[Cl:2][C:3]1[CH:36]=[CH:35][C:6]([CH2:7][CH:8]2[N:13]3[C:14](=[O:30])[CH:15]([N:29]4[CH:43]=[CH:47][CH:46]=[CH:45]4)[CH2:16][N:17]([S:18]([C:21]4[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=4[Cl:28])(=[O:20])=[O:19])[CH:12]3[CH2:11][N:10]([CH:31]([CH3:33])[CH3:32])[C:9]2=[O:34])=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 111,2-DichloroethaneHCID 790982,5-DimethoxytetrahydrofuranHCID 686934646-(4-Chlorobenzyl)-1-(2,4-dichlorobenzenesulfonyl)-3-amino-8-isopropylhexahydropyrazino[1,2-a]pyrimidine-4,7-dione hydrobromide

생성물 1

HCID 129914256-(4-Chlorobenzyl)-1-(2,4-dichlorobenzenesulfonyl)-8-isopropyl-3-pyrrol-1-ylhexahydropyrazino[1,2-a]pyrimidine-4,7-dione

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

64 mg of 6-(4-chlorobenzyl)-1-(2,4-dichlorobenzenesulfonyl)-3-amino-8-isopropylhexahydropyrazino[1,2-a]pyrimidine-4,7-dione hydrobromide (Example 2) were suspended in 1 ml of water, and 1 ml of DCE was added. This mixture was mixed with 2 equivalents of 2,5-dimethoxytetrahydrofuran and stirred at 80° C. for 1 hour. The DCE phase was removed and the aqueous phase was extracted twice with DCE. The combined extracts were evaporated, and the crude substance was dissolved in a mixture of acetonitrile and water and freeze dried. The pure title compound was removed after purification by HPLC. The system and process described under “general processes” was used for this. MW=608.08 (calculated, monoisotopic); measured value (M+H)+: 609.4.

후처리

  1. customThe DCE phase was removed
  2. extractionthe aqueous phase was extracted twice with DCE
  3. customThe combined extracts were evaporated
  4. dissolutionthe crude substance was dissolved in a mixture of acetonitrile and water and freeze
  5. customdried
  6. customThe pure title compound was removed
  7. customafter purification by HPLC

출처 및 근거

ORD 기록
ord-a887af8ca92441e1b2783f0fa69a8b06
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07652007B2

반응 노트

불러오는 중…