Benzyl 1-(2,6-dimethylpyrimidin-4-yl)piperidin-4-yl(methyl)carbamate → 1-(2,6-dimethylpyrimidin-4-yl)-N-methylpiperidin-4-amine

HRID 1193320노트

반응식

HRID 1193320 반응식
[CH3:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][CH:11]([N:14](C)[C:15](=O)OCC3C=CC=CC=3)[CH2:10][CH2:9]2)[CH:5]=[C:4]([CH3:26])[N:3]=1>CO>[CH3:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][CH:11]([NH:14][CH3:15])[CH2:10][CH2:9]2)[CH:5]=[C:4]([CH3:26])[N:3]=1

참가 물질

3

반응물 1

HCID 66798782Benzyl 1-(2,6-dimethylpyrimidin-4-yl)piperidin-4-yl(methyl)carbamate

생성물 1

HCID 470028741-(2,6-dimethylpyrimidin-4-yl)-N-methylpiperidin-4-amine수율 95%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Benzyl 1-(2,6-dimethylpyrimidin-4-yl)piperidin-4-yl(methyl)carbamate (3.6 g, 10.169 mmol, 1.0 eq.) was dissolved in MeOH (40 ml) and degassed for 15 min with N2. Pd(OH)2 (800 mg) was then added, and hydrogenation was carried out for 4 hours at room temperature under balloon pressure. After monitoring by TLC, the reaction mixture was filtered over Celite and washed with methanol (100 ml). The filtrate was concentrated under reduced pressure and the crude product was used in the next stage without being purified further. Yield: 95% (2.12 g, 9.636 mmol)

후처리

  1. customdegassed for 15 min with N2
  2. additionPd(OH)2 (800 mg) was then added
  3. filtrationthe reaction mixture was filtered over Celite
  4. washwashed with methanol (100 ml)
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customwithout being purified further

출처 및 근거

ORD 기록
ord-6abd554f6f9445149c13b9bc4a33761b
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680159B2

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