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

HRID 594062

反応式

HRID 594062 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4511474057dd4666a0129689127ff48e
出典データセット
uspto-grants-2016_01
特許番号
US09242969B2

関連ノート

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