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

HRID 1193320ノート

反応式

HRID 1193320 の反応式
[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

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-6abd554f6f9445149c13b9bc4a33761b
出典データセット
uspto-grants-2014_03
特許番号
US08680159B2

反応ノート

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