3-[6-Chloro-2-(4-nitro-phenyl)-pyrimidin-4-yl]-8-oxa-3-aza-bicyclo[3.2.1]octane → Isopropyl-[2-(4-nitro-phenyl)-6-(8-oxa-3-aza-bicyclo[3.2.1]oct-3-yl)-pyrimidin-4-yl]-amine

HRID 75415노트

반응식

HRID 75415 반응식
Cl[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=2)[N:5]=[C:4]([N:17]2[CH2:23][CH:22]3[O:24][CH:19]([CH2:20][CH2:21]3)[CH2:18]2)[CH:3]=1>C(N)(C)C>[CH:11]([NH:14][C:2]1[CH:3]=[C:4]([N:17]2[CH2:23][CH:22]3[O:24][CH:19]([CH2:20][CH2:21]3)[CH2:18]2)[N:5]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=2)[N:7]=1)([CH3:12])[CH3:10]

참가 물질

3

반응물 1

HCID 866658843-[6-Chloro-2-(4-nitro-phenyl)-pyrimidin-4-yl]-8-oxa-3-aza-bicyclo[3.2.1]octane

생성물 1

HCID 66750217Isopropyl-[2-(4-nitro-phenyl)-6-(8-oxa-3-aza-bicyclo[3.2.1]oct-3-yl)-pyrimidin-4-yl]-amine수율 198.3%

시약·촉매·용매 1

HCID 6363Isopropylamine용매

반응 조건

온도
140 °C

실험 절차

In a 2-5 mL microwave vial was placed 3-(6-chloro-2-(4-nitrophenyl)pyrimidin-4-yl)-8-oxa-3-azabicyclo[3.2.1]octane (13, 70 mg, 0.202 mmol) in iPrNH2 (4 ml) to give a yellow suspension. The reaction was heated under microwave irradiation at 140° C. for 90 min. The mixture was concentrated, dissolved in dichloromethane and washed with sat NaHCO3. The organic phase was dried over MgSO4, filtered and concentrated to give 74 mg of the title compound as a yellow solid (99%).

후처리

  1. customto give a yellow suspension
  2. concentrationThe mixture was concentrated
  3. dissolutiondissolved in dichloromethane
  4. washwashed
  5. dry with materialThe organic phase was dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fbe7ae7ed2ba4f29b4669ac13aad8e01
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835429B2

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