4-(4,6-Dichloropyrimidin-2-yl)morpholine → 4-(6-Chloropyrimidin-4-yl)morpholine

HRID 594055

반응식

HRID 594055 반응식
[Cl:1][C:2]1C=C(Cl)[N:5]=[C:4](N2CCOCC2)[N:3]=1.[NH:15]1[CH2:20][CH2:19]S(=O)(=O)[CH2:17][CH2:16]1.[CH3:23][CH2:24][OH:25].C1COCC1>>[Cl:1][C:2]1[N:3]=[CH:4][N:5]=[C:16]([N:15]2[CH2:23][CH2:24][O:25][CH2:19][CH2:20]2)[CH:17]=1

참가 물질

4

반응 조건

온도
100 °C

실험 절차

To a solution of 4-(4,6-dichloropyrimidin-2-yl)morpholine (1.0 equiv.) in EtOH:THF (1:1, 0.25 M) was added thiomorpholine 1,1-dioxide (1.0 equiv.) in one portion. The resulting mixture was heated to 100° C. for 42 h. The resulting mixture was then cooled to RT and concentrated in vacuo to yield an off white solid in The reaction mixture was then concentrated in vacuo and dried under high vacuum over 20 h to yield 4-(6-chloropyrimidin-4-yl)morpholine as a white solid in 97% yield. LCMS (m/z) (M+H)=333.0/334.9, Rt=0.68 min.

후처리

  1. temperatureThe resulting mixture was then cooled to RT
  2. concentrationconcentrated in vacuo
  3. customto yield an off white solid in The reaction mixture
  4. concentrationwas then concentrated in vacuo
  5. customdried under high vacuum over 20 h

출처 및 근거

ORD 기록
ord-8165ba03c8f2474a8cbd2fc4e09fe009
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242969B2

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