Isopropyl iodide → 1,1-Dimethylethyl 4-{[1-(1-methylethyl)-4-piperidinyl]methyl}-1-piperidinecarboxylate

HRID 1869621노트

반응식

HRID 1869621 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][CH:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)[CH2:3][CH2:2]1.[CH:21](I)([CH3:23])[CH3:22].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[CH3:22][CH:21]([N:1]1[CH2:2][CH2:3][CH:4]([CH2:7][CH:8]2[CH2:9][CH2:10][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:12][CH2:13]2)[CH2:5][CH2:6]1)[CH3:23]

참가 물질

5

반응물 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 497611974-Piperidin-4-ylmethyl-piperidine-1-carboxylic acid t-butyl ester

생성물 1

HCID 688888451,1-Dimethylethyl 4-{[1-(1-methylethyl)-4-piperidinyl]methyl}-1-piperidinecarboxylate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
50 °C

실험 절차

1,1-Dimethylethyl 4-(4-piperidinylmethyl)-1-piperidinecarboxylate (may be prepared as described in Description 2) (3 g), isopropyl iodide (3.2 ml) and K2CO3 (2.94 g) were combined in acetonitrile (70 ml) and the reaction mixture heated at 50° C. overnight. The reaction was allowed to cool to room temperature, filtered and evaporated. The residue was dissolved in diethylether (50 ml) and washed successively with water (50 ml), saturated sodium thiosulphate solution (50 ml), saturated brine (50 ml) and dried (Na2SO4). The solvent was evaporated to give the title compound (D3) as a pale yellow oil (3.1 g).

후처리

  1. temperatureto cool to room temperature
  2. filtrationfiltered
  3. customevaporated
  4. dissolutionThe residue was dissolved in diethylether (50 ml)
  5. washwashed successively with water (50 ml), saturated sodium thiosulphate solution (50 ml), saturated brine (50 ml)
  6. dry with materialdried (Na2SO4)
  7. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-64d3a6b4d34046f9998aafb24779ff0f
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07638631B2

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