Carbon Dioxide → HCID 59495804、化合物

HRID 219873

反応式

HRID 219873 の反応式
C([Li])(C)(C)C.Br[C:7]1[CH:12]=[CH:11][C:10]([N:13]2[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]2[CH3:19])=[C:9]([CH2:20][O:21][CH3:22])[CH:8]=1.[C:23](=[O:25])=[O:24]>CCOCC.CCOCC.CCOC(C)=O.O>[CH3:22][O:21][CH2:20][C:9]1[CH:8]=[C:7]([CH:12]=[CH:11][C:10]=1[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]1[CH3:19])[C:23]([OH:25])=[O:24]

参加物

7

反応物 3

HCID 280Carbon DioxideHCID 585541231-(4-Bromo-2-(methoxymethyl)phenyl)-2-methylpiperidineHCID 178418306HCID 178418306、化合物

生成物 1

HCID 59495804HCID 59495804、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒2 回HCID 21584169Diethylether ethylacetate溶媒

実験手順

To anhydrous Et2O (130 mL) at −78° C. was added tert-butyllithium (63.79 mL; 1.50 M; 95.68 mmol) (solution in pentane) which was followed by the slow addition of a solution of 1-[4-bromo-2-(methoxymethyl)phenyl]-2-methylpiperidine (12.97 g; 43.49 mmol) in anhydrous Et2O (20 mL). After 40 min, the reaction mixture was poured on an excess of freshly crushed dry ice and stirred for 30 min after which time it was diluted with Et2O/EtOAc (1:1, 800 mL), water (200 mL, pH 4-5). The organic layers were combined, dried over MgSO4 and the solvents were removed under reduced pressure to give a yellow oil that was triturated in iPr2O (˜20 mL) and pentane (˜20 mL), filtered off and washed with pentane to give the title compound as a beige powder. LC/MS (Method B): 264.1 (M+H)+.

後処理

  1. dry with materialdried over MgSO4
  2. customthe solvents were removed under reduced pressure
  3. customto give a yellow oil that
  4. customwas triturated in iPr2O (˜20 mL)
  5. filtrationpentane (˜20 mL), filtered off
  6. washwashed with pentane

出典と根拠

ORDレコード
ord-936a0edee15149f29d462b20cd920a2f
出典データセット
uspto-grants-2012_06
特許番号
US08202865B2

関連ノート

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