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CAS No. : | 452-79-9 | MDL No. : | MFCD00143162 |
Formula : | C7H6FI | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | XVHYSMVSLDIUCM-UHFFFAOYSA-N |
M.W : | 236.03 | Pubchem ID : | 2774524 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-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 |
---|---|---|
With 18-crown-6 ether; johnphos; sodium t-butanolate;tris-(dibenzylideneacetone)dipalladium(0); In tert-butyl alcohol; at 20℃; | Example 180 (5R)-7-(2-Fluoro-4-methylphenyl)-2-(trans-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-l- one H A mixture of (5R)-2-(fralphar°-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-l-one (20 mg, 0.00007 mol, this compound was prepared by using procedures analogous to those described in example 1, steps 1-5), 4-methyl-2-fluoro-l-iodobenzene (21 mg, 0.00009 mol), sodium tert-bvAoxide (9.98 mg, 0.000104 mol), 1,4,7,10,13,16-hexaoxacyclooctadecane (27.4 mg, 0.000104 mol) , 2-(di- tert-butylphosphino)biphenyl (0.8 mg, 0.000003 mol) , tris(diben2ylideneacetone)dipalladium(0) (1 mg, 0.000001 mol), in tert-butyl alcohol (1.0 mL, 0.010 mol) was stirred at rt for 18. The crude product was purified by prep-HPLC to afford the desired product. . LC-MS: 361.1 (MfH)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
69% | With potassium phosphate;copper(l) iodide; In ethylene glycol; butan-1-ol; at 100℃; | A mixture of (3S)-piperidin-3-ol hydrochloride (0.50 g, 0.0036 mol), 2-fluoro-l-iodo-4- methylbenzene (1.03 g, 0.00436 mol), copper(I) iodide (140 mg, 0.00073 mol), potassium phosphate (3.08 g, 0.0145 mol), and 1,2-ethanediol (0.810 mL, 0.0145 mol) in 1-butanol (7.28 mL, 0.0796 mol) <n="54"/>was heated at 100 0C under nitrogen for 2 nights. The reaction mixture was treated with water, and then extracted with EtOAc. The organic layers were combined, washed with brine, dried and evaporated to dryness. The residue was used directly in next step (519 mg, 69%). LCMS (M+H):210.2. |
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