Ethanol → 4-amino-4-methyl-N-(2-pyrimidinyl)piperidine

HRID 2055107ノート

反応式

HRID 2055107 の反応式
C(O)C.[NH2:4][C:5]1([CH3:11])[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1.Cl[C:13]1[N:18]=[CH:17][CH:16]=[CH:15][N:14]=1.C(=O)([O-])[O-].[K+].[K+]>O>[NH2:4][C:5]1([CH3:11])[CH2:10][CH2:9][N:8]([C:13]2[N:18]=[CH:17][CH:16]=[CH:15][N:14]=2)[CH2:7][CH2:6]1

参加物

6

反応物 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 744042-ChloropyrimidineHCID 210904454-Methylpiperidin-4-amine

生成物 1

HCID 218825664-amino-4-methyl-N-(2-pyrimidinyl)piperidine収率 65.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2 ml of an ethanol suspension containing 260 mg of 4-amino-4-methylpiperidine (synthesized according to a method described in U.S. Pat. No. 5,821,240), 237 mg of 2-chloropyrimidine and 858 mg of potassium carbonate was stirred at 50° C. for 12 hours. The reaction mixture was poured into water, and extracted with chloroform. The extract was washed with brine, dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. The residue was purified by silica gel flash column chromatography [solvent: chloroform-methanol-aqueous ammonia (300:10:1)] to obtain 259 mg of 4-amino-4-methyl-N-(2-pyrimidinyl)piperidine (Reference Example 8-1 in Table 9).

後処理

  1. customsynthesized
  2. extractionextracted with chloroform
  3. washThe extract was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified by silica gel flash column chromatography [solvent: chloroform-methanol-aqueous ammonia (300:10:1)]

出典と根拠

ORDレコード
ord-a09c43af4c764edeb673678484eda59f
出典データセット
uspto-grants-2008_02
特許番号
US07332487B2

反応ノート

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