Ethyl Acetate → 2-tert-Butoxy-4-[2-[4-(2-fluorophenoxymethyl)piperidino]ethyl]pyrimidine

HRID 606219노트

반응식

HRID 606219 반응식
[C:1]([O:5][C:6]1[N:11]=[C:10]([CH:12]=[CH2:13])[CH:9]=[CH:8][N:7]=1)([CH3:4])([CH3:3])[CH3:2].Cl.[F:15][C:16]1[CH:29]=[CH:28][CH:27]=[CH:26][C:17]=1[O:18][CH2:19][CH:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>C(O)C>[C:1]([O:5][C:6]1[N:11]=[C:10]([CH2:12][CH2:13][N:23]2[CH2:22][CH2:21][CH:20]([CH2:19][O:18][C:17]3[CH:26]=[CH:27][CH:28]=[CH:29][C:16]=3[F:15])[CH2:25][CH2:24]2)[CH:9]=[CH:8][N:7]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 171780504-((2-Fluorophenoxy)methyl)piperidine hydrochlorideHCID 222481652-Tert-butoxy-4-vinylpyrimidine

생성물 1

HCID 222479962-tert-Butoxy-4-[2-[4-(2-fluorophenoxymethyl)piperidino]ethyl]pyrimidine수율 93%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

After dissolving 221 mg of 2-tert-butoxy-4-vinylpyrimidine and 200 mg of 4-(2-fluorophenoxymethyl)piperidine hydrochloride in 5 ml of ethanol, 123 mg of anhydrous potassium carbonate was added and the mixture was heated to reflux for 50 minutes. Ethyl acetate was added to the reaction mixture, the insoluble portion was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by NH silica gel column chromatography (solvent: n-hexane/ethyl acetate) to obtain the title compound (293 mg, 93% yield).

후처리

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 50 minutes
  4. filtrationthe insoluble portion was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by NH silica gel column chromatography (solvent: n-hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-2db74d89b0974e5d91c9442f241f260d
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915274B2

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