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Sodium Methoxide → HCID 69431484, 화합물

HRID 1592854
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HRID 1592854 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][N:15]([C:17]2[CH:22]=[CH:21][N:20]=[C:19]([Cl:23])[N:18]=2)[CH3:16])[CH2:10][CH2:9]1)=O)(C)(C)C.[CH3:24][O-:25].[Na+]>CO>[ClH:23].[CH3:24][O:25][C:19]1[N:18]=[C:17]([N:15]([CH2:14][CH:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)[CH3:16])[CH:22]=[CH:21][N:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 71647831544696-02-8

생성물 1

HCID 69431484HCID 69431484, 화합물수율 130.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A stirred suspension of 1-t-butoxycarbonyl-4-{[(2-chloropyrimidin-4-yl)(methyl)amino]methyl}piperidine (1.00 g, 2.93 mmol) and sodium methoxide (633 mg, 11.7 mmol) in methanol (7.3 mL) is heated under reflux for 48 hours. Excess methanol is removed in vacuo and the residue is taken into water and ethyl acetate. The phases are separated and the aqueous phase is extracted into ethyl acetate (×3). The combined organic extracts are dried (sodium sulfate), filtered and concentrated in vacuo. The residue is taken into methanol (100 mL) and hydrogen chloride gas is passed through the solution maintaining <20° C. The mixture is kept at this temperature for 2 hours before it is concentrated in vacuo giving 4-{[(2-methoxypyrimidin-4-yl)(methyl)amino]methyl}piperidine hydrochloride (1.04 g, 100%).

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 48 hours
  3. customExcess methanol is removed in vacuo
  4. customThe phases are separated
  5. extractionthe aqueous phase is extracted into ethyl acetate (×3)
  6. dry with materialThe combined organic extracts are dried (sodium sulfate)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. temperaturemaintaining <20° C
  10. concentrationis concentrated in vacuo

출처 및 근거

ORD 기록
ord-782cf752fa8749e18f35955d1146ec8a
출처 데이터셋
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07294627B2

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