Diisopropylethylamine → HCID 67343276, 화합물

HRID 451412

반응식

HRID 451412 반응식
[C:1]([N:8]1CCC(N)C[CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].Cl[C:16]1[CH:21]=[C:20]([CH3:22])[N:19]=[CH:18][N:17]=1.C([N:26]([CH2:30][CH3:31])[CH:27]([CH3:29])C)(C)C>O1CCOCC1.O>[C:4]([O:3][C:1](=[O:2])[NH:8][CH:9]1[CH2:29][CH2:27][N:26]([C:16]2[CH:21]=[C:20]([CH3:22])[N:19]=[CH:18][N:17]=2)[CH2:30][CH2:31]1)([CH3:7])([CH3:6])[CH3:5]

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 5817964-Chloro-6-methylpyrimidineHCID 12682914-Amino-1-Boc-piperidine

생성물 1

HCID 67343276HCID 67343276, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

반응 조건

온도
150 °C

실험 절차

A suspension of Boc-4-aminopiperidine (613 mg, 3 mmol), 4-chloro-6-methylpyrimidine (433 mg, 3.3 mmol) and N,N-diisopropylethyl amine (771 L, 4.5 mmol) in dioxane (12 mL) was heated to 150° C. in the microwave for 30 minutes. The reaction was diluted with water and extracted twice with ethyl acetate. The combined organic layers were washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel using a gradient from AcOEt to AcOEt/EtOH 9:1 as eluent. The title compound was obtained as a light yellow solid (693 mg, 79%).

후처리

  1. extractionextracted twice with ethyl acetate
  2. washThe combined organic layers were washed with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude product was purified by column chromatography on silica gel using a gradient from AcOEt to AcOEt/EtOH 9:1 as eluent

출처 및 근거

ORD 기록
ord-6de883d95cf14582bc0237df04c0840d
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

연결된 노트

불러오는 중…