4-(N-Boc-amino)piperidine → HCID 86608254, 화합물

HRID 2233860노트

반응식

HRID 2233860 반응식
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]

참가 물질

4

반응물 2

HCID 7238334-(N-Boc-amino)piperidineHCID 13447564N-[6-Chloro-2-(methylsulfanyl)pyrimidin-4-yl]acetamide2회

생성물 1

HCID 86608254HCID 86608254, 화합물수율 93.8%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-aea0fc5df0d64898b667f0ef62ea0015
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709503B2

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