Aluminium lithium hydride → 1-[2-(2-Fluorophenoxy)-ethyl]-4-[3-(3,4,5-trimethoxyphenyl)propyl]-piperazine dihydrochloride

HRID 1928548

반응식

HRID 1928548 반응식
[ClH:1].[F:2][C:3]1[CH:33]=[CH:32][CH:31]=[CH:30][C:4]=1[O:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][N:11]([C:14](=O)[CH2:15][CH2:16][C:17]2[CH:22]=[C:21]([O:23][CH3:24])[C:20]([O:25][CH3:26])=[C:19]([O:27][CH3:28])[CH:18]=2)[CH2:10][CH2:9]1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[ClH:1].[ClH:1].[F:2][C:3]1[CH:33]=[CH:32][CH:31]=[CH:30][C:4]=1[O:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][C:17]2[CH:22]=[C:21]([O:23][CH3:24])[C:20]([O:25][CH3:26])=[C:19]([O:27][CH3:28])[CH:18]=2)[CH2:10][CH2:9]1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 672988021-{4-[2-(2-Fluorophenoxy)ethyl]piperazin-1-yl}-3-(3,4,5-trimethoxyphenyl)propan-1-one hydrochloride

생성물 1

HCID 672992191-[2-(2-Fluorophenoxy)-ethyl]-4-[3-(3,4,5-trimethoxyphenyl)propyl]-piperazine dihydrochloride수율 173.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 1-{4-[2-(2-fluorophenoxy)ethyl]piperazin-1-yl}-3-(3,4,5-trimethoxyphenyl)-propan-1-one hydrochloride (0.2 g, 0.41 mmol) in THF (50 mL) was added LiAlH4 (0.2 g, 5 mmol). The reaction mixture was stirred under N2 for a day, cooled with an ice bath, and quenched with water (0.2 mL) and 10N NaOH aqueous solution (0.2 mL). The solid was filtered and the filtrate was concentrated to dryness. The residue was treated with ether and 2N HCl in ether (2 mL). The white solid was filtered and dried under vacuum to yield the title compound (0.18 g, 87%).

후처리

  1. temperaturecooled with an ice bath
  2. customquenched with water (0.2 mL) and 10N NaOH aqueous solution (0.2 mL)
  3. filtrationThe solid was filtered
  4. concentrationthe filtrate was concentrated to dryness
  5. additionThe residue was treated with ether and 2N HCl in ether (2 mL)
  6. filtrationThe white solid was filtered
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-51b4db710de04d45974849d18197797c
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183374B2

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