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CAS No. : | 22013-33-8 | MDL No. : | MFCD00006824 |
Formula : | C8H9NO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | BZKOZYWGZKRTIB-UHFFFAOYSA-N |
M.W : | 151.16 | Pubchem ID : | 89148 |
Synonyms : |
|
Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H312-H315-H319-H332-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
94% | In ethanol; water;Heating / reflux; | A solution of l-oxa-spiro[2.5]octane-6-carboxylic acid ethyl ester obtained according to Tetrahedron, 1995, 51, 10259-80, (4.5 g, 24.4 mmol) and 2,3-dihydro-benzo[l,4]dioxin- 6-ylamine (3.7 g, 24.4 mmol) in EtOH/water (9:1, 100 ml) was heated at reflux overnight. The mixture was concentrated in vacuo and purified by chromatography (Hex:EA 2:1) to give the title amino alcohols (7.7 g, 94% yield) as an orange oil.1H NMR (DMSO d6) delta: 6.60-6.50 (m, IH); 6.20-6.10 (m, 2H); 5.90-5.70 (m, IH); 4.10-3.90 (m, 6H); 3.90-3.80 (m, 2H); 2.40-2.20 (m, IH); 1.80-1.40 (m, 7H), 1.40-1.20 (m, 2H); 1.10-1.00 (m, 4H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
87% | In ethanol; for 3h;Reflux; | General procedure: The appropriate amine (10 mmol) was heated at reflux with the appropriate aldehyde (10 mmol) in ethanol (50 mL) for 3 h. The reaction mixture was cooled and then the solvent evaporated in vacuo. The resulting solid product was recrystallised from ethanol. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 60℃; | General procedure: A solution of <strong>[848398-41-4]2,4-dichloro-5,7-dihydrofuro[3,4-d]pyrimidine</strong> (4, 1.89g, 10mmol) in DMSO (10mL) was added commercially available 3,4-dimethoxyaniline (1.53g, 10mmol) and DIPEA (2.58g, 20mmol). The solution was heated to 60C and stirred overnight. Then the solution was poured into water and extracted with EtOAc, the organic layer was washed by brine, dried with anhydrous Na2SO4, and filtered and concentrated under reduced pressure. The crude product was further purified by flash chromatography on silica gel (EtOAc/hexane=1:1) to afford 8 compound 5 (2.00g, yield 65%) as an off-white solid. 1H NMR (400MHz, CDCl3) delta: 6.90-6.81 (m, 3H), 4.88 (s, 2H), 4.42 (s, 2H), 3.92 (s, 3H), 3.89 (s, 3H). |
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