4-(N-Boc-amino)piperidine → HCID 86608254、化合物

HRID 2233860ノート

反応式

HRID 2233860 の反応式
Cl[C:2]1[N:7]=[C:6]([S:8][CH3:9])[N:5]=[C:4]([NH:10][C:11](=[O:13])[CH3:12])[CH:3]=1.[NH:14]1[CH2:19][CH2:18][CH:17]([NH:20][C:21](=[O:27])[O:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:16][CH2:15]1>CN1C(=O)CCC1>[C:11]([NH:10][C:4]1[N:5]=[C:6]([S:8][CH3:9])[N:7]=[C:2]([N:14]2[CH2:15][CH2:16][CH:17]([NH:20][C:21](=[O:27])[O:22][C:23]([CH3:25])([CH3:24])[CH3:26])[CH2:18][CH2:19]2)[CH:3]=1)(=[O:13])[CH3:12]

参加物

4

反応物 2

HCID 7238334-(N-Boc-amino)piperidineHCID 13447564N-[6-Chloro-2-(methylsulfanyl)pyrimidin-4-yl]acetamide2 回

生成物 1

HCID 86608254HCID 86608254、化合物収率 93.8%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

TEA (0.32 ml, 2.28 mmol) and N-[6-chloro-2-(methylthio)pyrimidin-4-yl]acetamide (Intermediate 44, 0.50 g, 2.28 mmol) were added to a solution of tert-butyl piperidin-4-ylcarbamate (0.46 g, 2.28 mmol) in NMP (2 ml) at room temperature. Using a Smith Microwave Synthesizer, the mixture was subjected to single-mode microwave at 150° C. for 10 minutes. The mixture was partitioned between water and EtOAc. The layers were separated and the organic layer was washed with water two more times. The organic phase was dried over magnesium sulfate and concentrated to give the title compound (816 mg).

後処理

  1. customat 150° C.
  2. customfor 10 minutes
  3. customThe mixture was partitioned between water and EtOAc
  4. customThe layers were separated
  5. washthe organic layer was washed with water two more times
  6. dry with materialThe organic phase was dried over magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-aea0fc5df0d64898b667f0ef62ea0015
出典データセット
uspto-grants-2010_05
特許番号
US07709503B2

反応ノート

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