Morpholine → HCID 90408881, 화합물

HRID 594091노트

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HRID 594091 반응식
Cl[C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([Cl:10])[N:3]=1.[NH:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1>>[Cl:10][C:4]1[N:3]=[C:2]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=1

참가 물질

3

반응물 2

HCID 8083MorpholineHCID 33199932,6-Dichloro-4-methoxypyridine

생성물 1

HCID 90408881HCID 90408881, 화합물수율 43%

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온도
130 °C

실험 절차

A mixture of 2,6-dichloro-4-methoxypyridine (1.0 equiv.) and morpholine (20 equiv.) were heated to 130° C. for 40 min in the microwave. The reaction mixture was centrifuged and the soluble portion was removed from solids. Water was added to the soluble portion which resulted in precipitation of product. This mixture was centrifuged and the soluble portion was discarded. The remaining solids were partitioned between water and EtOAc. The organic phase was washed with brine and dried over sodium sulfate. The solution was concentrated and dried under vacuo to give 4-(6-chloro-4-methoxypyridin-2-yl)morpholine in 43% yield. LCMS (m/z) (M+H)=229.1, Rt=0.76 min.

후처리

  1. customthe soluble portion was removed from solids
  2. additionWater was added to the soluble portion which
  3. customresulted in precipitation of product
  4. customThe remaining solids were partitioned between water and EtOAc
  5. washThe organic phase was washed with brine
  6. dry with materialdried over sodium sulfate
  7. concentrationThe solution was concentrated
  8. customdried under vacuo

출처 및 근거

ORD 기록
ord-e392d44616374ad7a54aaabd9a86622b
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242969B2

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