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

HRID 1869621ノート

反応式

HRID 1869621 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
50 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-64d3a6b4d34046f9998aafb24779ff0f
出典データセット
uspto-grants-2009_12
特許番号
US07638631B2

反応ノート

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