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

HRID 722019

반응식

HRID 722019 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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)]

출처 및 근거

ORD 기록
ord-053d787a165944de89f3ae46539e47f4
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138397B2

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