Aluminium lithium hydride → HCID 68691037, 화합물

HRID 1159092노트

반응식

HRID 1159092 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[CH:31]=[C:30]([O:32][CH3:33])[CH:29]=[CH:28][C:10]=1[CH2:11][N:12]1[C:25](=O)[CH:24]([CH3:27])[N:15]2[CH2:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:22]=3[CH2:23][C@@H:14]2[CH2:13]1>C1COCC1>[CH3:7][O:8][C:9]1[CH:31]=[C:30]([O:32][CH3:33])[CH:29]=[CH:28][C:10]=1[CH2:11][N:12]1[CH2:25][CH:24]([CH3:27])[N:15]2[CH2:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:22]=3[CH2:23][C@@H:14]2[CH2:13]1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 68687822HCID 68687822, 화합물

생성물 1

HCID 68691037HCID 68691037, 화합물수율 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Lithium aluminum hydride (1 M in THF, 0.63 ml, 0.63 mmol) was added to a solution of (11aR)-1,2,11,11a-tetrahydro-2-(2,4-dimethoxybenzyl)-4-methyl-4H-pyrazino[1,2-b]isoquinolin-3(6H)-one (0.11 g, 0.31 mmol) in THF (1.8 ml) stirring in a room temperature bath under nitrogen. After stirring at 65° C. for 2 h, the reaction was cooled to room temperature and slowly quenched with water (0.18 ml). Sodium hydroxide (1N, 0.36 ml) followed by water (0.27 ml) were then added and the resultant gelatinous precipitate was filtered through Celite® rinsing THF. The filtrate after evaporation of the solvent was transferred to a separatory funnel with EtOAc. Washing with brine and drying with MgSO4 afforded crude product (0.10 g, 95% yield) after evaporation of the solvent. This material was used in the next step without further purification.

후처리

  1. stirringAfter stirring at 65° C. for 2 h
  2. temperaturethe reaction was cooled to room temperature
  3. customslowly quenched with water (0.18 ml)
  4. additionwere then added
  5. filtrationthe resultant gelatinous precipitate was filtered through Celite®
  6. washrinsing THF
  7. customThe filtrate after evaporation of the solvent
  8. customwas transferred to a separatory funnel with EtOAc
  9. washWashing with brine
  10. dry with materialdrying with MgSO4

출처 및 근거

ORD 기록
ord-95b4833c41e14b6dadd38e7476aa4da1
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812024B2

반응 노트

불러오는 중…