1,1'-Carbonyldiimidazole → HCID 69662350, 화합물
반응식
[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]1참가 물질
4
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-1ce519a6f46d472ab6a37ab909b785f8
- 출처 데이터셋
- uspto-grants-2003_05
- 특허 번호
- US06559162B2
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