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Triethylamine → 4-(6-Chloro-2-morpholinopyrimidin-4-yl)-2,2-dimethylmorpholine

HRID 594062
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HRID 594062 반응식
[CH3:1][C:2]1([CH3:8])[O:7][CH2:6][CH2:5][NH:4][CH2:3]1.[Cl:9][C:10]1[CH:15]=[C:14](Cl)[N:13]=[C:12]([N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[N:11]=1.C(N(CC)CC)C>CCO>[Cl:9][C:10]1[N:11]=[C:12]([N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[N:13]=[C:14]([N:4]2[CH2:5][CH2:6][O:7][C:2]([CH3:8])([CH3:1])[CH2:3]2)[CH:15]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27720684-(4,6-Dichloropyrimidin-2-yl)morpholineHCID 189596742,2-Dimethylmorpholine

생성물 1

HCID 904095494-(6-Chloro-2-morpholinopyrimidin-4-yl)-2,2-dimethylmorpholine

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
110 °C

실험 절차

A mixture of 2,2-dimethylmorpholine (2.0 equiv.), 4-(4,6-dichloropyrimidin-2-yl)morpholine (1 equiv.) and triethylamine (6 equiv.) in EtOH (0.2 M) were heated to 110° C. for 25 min in the microwave. The reaction mixture was partitioned between EtOAc and water. The organic phase was dried over sodium sulfate. The resulting solution was concentrated and dried under vacuo to give 4-(6-chloro-2-morpholinopyrimidin-4-yl)-2,2-dimethylmorpholine and was used in the next step without further purification. LCMS (m/z) (M+H)=313.2, Rt=0.86 min.

후처리

  1. customThe reaction mixture was partitioned between EtOAc and water
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. concentrationThe resulting solution was concentrated
  4. customdried under vacuo

출처 및 근거

ORD 기록
ord-4511474057dd4666a0129689127ff48e
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09242969B2

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