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CAS No. : | 33821-94-2 | MDL No. : | MFCD00058593 |
Formula : | C8H15BrO2 | Boiling Point : | - |
Linear Structure Formula : | Br(CH2)3OC5H9O | InChI Key : | HJNHUFQGDJLQRS-UHFFFAOYSA-N |
M.W : | 223.11 | Pubchem ID : | 2777988 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | N/A |
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 |
---|---|---|
62% | EXAMPLE 50 6-Bromo-4-[3-(tetrahydro-pyran-2-yloxy)-propoxy]-1-benzopyran-2-one 6-Bromo-4-hydroxycoumarin (1.19 mmol, 0.287 g), K2CO3 (3.57 mmol, 0.493 g) and 2-3-(bromopropoxy)tetrahydro-2H-pyran (1.19 mmol, 0.264 g) is suspended in 10 mL of acetone, and is heated to 55 C. for 24 hrs at which time the reaction is not complete. Cs2CO3 (1.54 mmol, 0.5 g) and 5 mL of DMF are added and the reaction is heated for an additional 2 hrs. Twenty-five percent of the crude THP protected material is purified by HPLC to afford the title compound (70.8 mg, 62%); 1H NMR (CDCl3, 300 MHz) delta 7.91 (1H, d, J=2.25 Hz), 7.82 (1H, dd, J=2.5, 9 Hz), 7.39 (1H, d, J=9 Hz), 5.98 (1H, s), 4.59 (1H, m), 4.31 (2H, t, J=6 Hz), 3.83 (1H, m), 3.72 (1H, m), 3.55 (2H, m), 2.09 (2H, m), 1.65 (2H, m), 1.45 (4H, m); MS (ESI, Pos.) calcd for C17H19BrO5 m/z [M+H]=383.0, found 383.1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: (a) Alkylation and Suzuki coupling in one pot: A mixture of 0.58 mmol of halogen derivative 23 or 24, 100 mg (0.72 mmol, 1.2 equiv) of K2CO3 and 3 mL of DMF was stirred in a 100 C oil bath for 30 min, cooled to rt, and treated with alkylating reagent (1.2 equiv to halogen derivative). The resulting mixture was subjected to microwave reactor at 110 C for 10,000 s, cooled to rt, charged with a mixture of boronic acid (1.2 equiv to halogen derivative), 115 mg of K2CO3 (1.2 equiv to boronic acid), and 15 mg of PdCl2, and again subjected to microwave reactor at 130 C for 35 min. The resulting suspension was evaporated to dryness. The residue was adsorbed on silica gel and purified by standard flash chromatography method with MeOH and DCM to give the crude product (bearing protected and unprotected hydroxyls) as a mixture. |
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