Morpholine → 4-(6-Chloropyrimidin-4-yl)morpholine

HRID 594054

반응식

HRID 594054 반응식
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][N:3]=1.[NH:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1.C(N(CC)CC)C>CCO>[Cl:8][C:6]1[N:5]=[CH:4][N:3]=[C:2]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)[CH:7]=1

참가 물질

5

반응물 3

HCID 8083MorpholineHCID 8471TriethylamineHCID 709434,6-Dichloropyrimidine

생성물 1

HCID 7960704-(6-Chloropyrimidin-4-yl)morpholine수율 93%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 4,6-dichloropyrimidine (1.0 equiv.) in EtOH (0.44 M) was added morpholine (1.0 equiv.) followed by triethylamine (1.10 equiv.). The resulting mixture was stirred at RT for 16 hours. 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 93% yield. LCMS (m/z) (M+H)=200.0/201.8, Rt=0.35 min. 1H NMR (400 MHz, <cdcl3>) δ ppm 3.53-3.71 (m, 4H) 3.72-3.83 (m, 4H) 6.51 (s, 1H) 8.39 (s, 1H) 11.75 (br. s., 1H).

후처리

  1. concentrationThe reaction mixture was then concentrated in vacuo
  2. customdried under high vacuum over 20 h

출처 및 근거

ORD 기록
ord-e9f4c71f8d474a7d929dd8217a406dec
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242969B2

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