1,1'-Carbonyldiimidazole → HCID 69662350、化合物
反応式
[C:1]([O:4][CH2:5][C:6]([OH:9])([CH3:8])[CH3:7])(=[O:3])[CH3:2].[C:10](N1C=CN=C1)([N:12]1[CH:16]=[CH:15][N:14]=[CH:13]1)=[O:11]>C(Cl)Cl>[N:12]1([C:10]([O:9][C:6]([CH3:8])([CH3:7])[CH2:5][O:4][C:1](=[O:3])[CH3:2])=[O:11])[CH:16]=[CH:15][N:14]=[CH:13]1参加物
4
実験手順
A mixture of 2-hydroxy-2-methylpropyl acetate (3.35 g, 25.3 mmol) and 1,1′-carbonyldiimidazole (4.11 g, 25.3 mmol) in DCM was stirred for 8 h at rt. The mixture was then transferred to a closed vessel and heated to 100° C. overnight. The mixture was concentrated in vacuo before ether and water were added. The organic phase was separated, dried and concentrated in vacuo. The resulting residue was purified by chromatography on silica gel, eluting with THF:heptane (1:1), to give the title compound in 20% yield.
後処理
- customThe mixture was then transferred to a closed vessel
- temperatureheated to 100° C. overnight
- concentrationThe mixture was concentrated in vacuo before ether and water
- additionwere added
- customThe organic phase was separated
- customdried
- concentrationconcentrated in vacuo
- customThe resulting residue was purified by chromatography on silica gel
- washeluting with THF:heptane (1:1)
出典と根拠
- ORDレコード
- ord-d1c66f5f4c4545aa97dfd233f1fa1167
- 出典データセット
- uspto-grants-2006_12
- 特許番号
- US07144914B2
反応ノート
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