Morpholine → 4-(4-(Benzyloxy)-6-chloropyridin-2-yl)morpholine

HRID 594093

反応式

HRID 594093 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[C:13](Cl)[N:12]=[C:11]([Cl:16])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1>CN1C(=O)CCC1>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([Cl:16])[N:12]=[C:13]([N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 8083MorpholineHCID 582090464-(Benzyloxy)-2,6-dichloropyridine

生成物 1

HCID 904099474-(4-(Benzyloxy)-6-chloropyridin-2-yl)morpholine

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
130 °C

実験手順

A mixture of 4-(benzyloxy)-2,6-dichloropyridine (1.0 equiv.) and morpholine (1.2 equiv.) in NMP (2 M) were heated to 130° C. for 1 h in the microwave. The reaction mixture was 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 crude 4-(4-(benzyloxy)-6-chloropyridin-2-yl)morpholine and was used in the next step without further purification. LCMS (m/z) (M+H)=305.0, Rt=1.10 min.

後処理

  1. customThe reaction mixture was partitioned between water and EtOAc
  2. washThe organic phase was washed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationThe solution was concentrated
  5. customdried under vacuo

出典と根拠

ORDレコード
ord-c2eedfd2ac7642efb0746d80526589d0
出典データセット
uspto-grants-2016_01
特許番号
US09242969B2

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