Ammonium Chloride → 1-(1-Benzyl-4-methyl-piperidin-4-yl)-4-methyl-piperazine

HRID 730633노트

반응식

HRID 730633 반응식
C[Mg]Cl.[CH2:4]([N:11]1[CH2:16][CH2:15][C:14]([N:19]2[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]2)([C:17]#N)[CH2:13][CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[NH4+].[Cl-]>C1COCC1>[CH2:4]([N:11]1[CH2:16][CH2:15][C:14]([N:19]2[CH2:20][CH2:21][N:22]([CH3:25])[CH2:23][CH2:24]2)([CH3:17])[CH2:13][CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 579896001-Benzyl-4-(4-methyl-piperazin-1-yl)-piperidin-4-carbonitrileHCID 178418332HCID 178418332, 화합물

생성물 1

HCID 672729861-(1-Benzyl-4-methyl-piperidin-4-yl)-4-methyl-piperazine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

10 mL methylmagnesium chloride solution (30 mmol, 3 M in THF) were added at RT to a solution of 3.0 g (10.1 mmol) 1-benzyl-4-(4-methyl-piperazin-1-yl)-piperidin-4-carbonitrile in 50 mL dry THF and the reaction mixture was stirred for 2 h. It was combined with saturated NH4Cl solution, stirred for 10 min, extracted exhaustively with diethyl ether and the combined organic phases were dried on Na2SO4. After the elimination of the desiccant and solvent the residue was purified by chromatography (Alox, activity stage II-III, gradient DCM/MeOH 100:1 to 50:1).

후처리

  1. stirringstirred for 10 min
  2. extractionextracted exhaustively with diethyl ether
  3. customthe combined organic phases were dried on Na2SO4
  4. customAfter the elimination of the desiccant and solvent the residue was purified by chromatography (Alox, activity stage II-III, gradient DCM/MeOH 100:1 to 50:1)

출처 및 근거

ORD 기록
ord-69d99ebcf57a4ac9a07f32495699c289
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582625B2

반응 노트

불러오는 중…