1,1'-Carbonyldiimidazole → HCID 178505196、化合物

HRID 1890357ノート

反応式

HRID 1890357 の反応式
[CH3:1][S:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]([NH2:12])=[C:8]([NH:13][CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[N:7]=1)(=[O:4])=[O:3].C1N=CN([C:25](N2C=NC=C2)=[O:26])C=1>C1COCC1>[CH3:1][S:2]([O:5][C:6]1[N:7]=[C:8]2[N:13]([CH:14]3[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]3)[C:25]([OH:26])=[N:12][C:9]2=[CH:10][CH:11]=1)(=[O:3])=[O:4]

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 866552605-Amino-6-(cyclohexylamino)pyridin-2-yl Methanesulfonate

生成物 1

HCID 178505196HCID 178505196、化合物収率 61.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

5-Amino-6-(cyclohexylamino)pyridin-2-yl methanesulfonate (1.44 g, 5.05 mmol) was dissolved in THF (30 mL) and CDI (2.455 g, 15.14 mmol) was added. The mixture was heated at 70° C. for 3 h. THF was removed and the residue was dissolved in EtOAc. The resulting solution was washed with water followed by 1 M HCl, dried over MgSO4 and concentrated under reduced pressure to give the title compound (0.96 g) without further purification. LCMS m/z=312.50 [M+H]+.

後処理

  1. customTHF was removed
  2. dissolutionthe residue was dissolved in EtOAc
  3. washThe resulting solution was washed with water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d8bd6f6e32274b07b4ba1a291671ebb3
出典データセット
uspto-grants-2013_08
特許番号
US08507473B2

反応ノート

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