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CAS No. : | 56990-02-4 | MDL No. : | MFCD00156887 |
Formula : | C7H4Br2O | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | ZLDMZIXUGCGKMB-UHFFFAOYSA-N |
M.W : | 263.91 | Pubchem ID : | 622077 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P301+P312-P302+P352-P304+P340-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-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 |
---|---|---|
84% | With sodium tetrahydroborate; In methanol; at 0 - 20℃; for 1h; | Example 15 [4-[3,5-Bis-[(4-trifluoromethylphenyl)ethynyl]benzyloxy]-2-methylphenoxy]acetic acid 3,5-Dibromobenzaldehyde (1.7 g, 6.3 mmol) was dissolved in methanol (100 mL) and sodium borohydride (0.250 g, 6.3 mmol) was added at 0° C. The reaction mixture was stirred for 0.5 h at 0° C. and then at 20° C. for another 0.5 h. The reaction mixture was concentrated in vacuo, diluted with brine (250 mL), acidified with hydrochloric acid and extracted with dichloromethane (3*50 mL). Evaporation of the organic solution gave 3,5-dibromo-benzyl alcohol as a white crystalline compound. Yield: 1.4 g (84percent). RF (SiO2, hexanes/ethyl acetate 9:1) 0.25. 1H NMR spectrum (300 MHz, CDCl3, A) 7.59 (d, J=1.5 Hz, 1H); 7.47 (d, J=1.5 Hz, 2H); 4.36 (s, 2H); 1.55 (s, 1H). |
84% | With sodium tetrahydroborate; In methanol; at 0 - 20℃; for 1h; | Example 15; [4-[3,5-Bis-[(4-trifluoromethylphenyl)ethynyl]benzyloxy]-2-methylphenoxy]acetic acid; 3,5-Dibromobenzaldehyde (1.7 g, 6.3 mmol) was dissolved in methanol (100 mL) and sodium borohydride (0.250 g, 6.3 mmol) was added at 0 °C. The reaction mixture was stirred for 0.5 h at 0 °C and then at 20 °C for another 0.5 h. The reaction mixture was con- centrated in vacuo, diluted with brine (250 mL), acidified with hydrochloric acid and extracted with dichloromethane (3 x 50 mL). Evaporation of the organic solution gave 3,5-dibromo- benzyl alcohol as a white crystalline compound. Yield: 1.4 g (84 percent). RF (Si02, hexanes/ethyl acetate 9:1) 0.25. 1H NMR spectrum (300 MHz, CDCl3, No.H) : 7.59 (d, J=1.5 Hz, 1 H) ; 7.47 (d, J=1.5 Hz, 2 H); 4.36 (s, 2 H); 1.55 (s, 1 H). |
With sodium borohydrid; In methanol; | PREPARATION 9 3,5-Dibromobenzyl alcohol Sodium borohydride (0.75 g) was added portionwise to a stirred suspension of 3,5-dibromobenzaldehyde (10.46 g) in methanol (50 ml) at 0° C. The mixture was stirred at 0° C. for 30 minutes, allowed to warm to room temperature and then its pH was adjusted to 2 using concentrated hydrochloric acid. Evaporation under vacuum provided a residue which was partitioned between ethyl acetate and water. The organic phase was washed with water, dried (MgSO4), then evaporated under vacuum to furnish the title compound as a solid (10.0 g), m.p. 103°-104° C. Found: C,31.98; H,2.23. C7 H6 Br2 O requires C,31.61; H,2.77percent. |
Example 1.1.76: (3-isopropyl-5-(methylsulfonylmethyl)phenyl)methanamine; To stirring solution of 5.0 g (18.9 mmol) of 3,5-dibromobenzaldehyde in 30 mL of MeOH and 25 mL of THF at 0 0C was added 819 mg of NaBH4 in 3 portions. The yellow solution was stirred at 0 0C for 30 min. and then concentrated. Water and EtOAc were added, and 1 N HCl was added to a pH = 7. The organic layer was washed with 25 mL of brine, dried over Na2SO4, filtered, and concentrated. (3,5-dibromophenyl)methanol was used in the next reaction without further purification. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With pyridine; copper(l) cyanide; In DMF (N,N-dimethyl-formamide); at 140℃; | A mixture of 3, [5-DIBROMOBENZALDEHYDE] (1 [G),] copper cyanide (0.331 [G)] and pyridine (0.3 mL) in DMF (30 mL) was heated to [140C] overnight. The solution was allowed to cool to r. t. and dropped into water (30 [ML),] then exctracted with Et20 (15 mL). The organic phase was dried, concentrated in vacuo and the residue was purified by flash chromatography (CH, [CH/ACOET FROM] 95: 5 to 80: 20) to give the title compound (64 mg) as a yellow oil. T. I. c.: CH/AcOEt [8] : 2, Rf=0.52 (detection with 2, [4-DINITROPHENYLHYDRAZINE).] NMR [(CDCI3)] : [6] (ppm) 10.0 (s, [1H)] ; 8.20 (s, [1H)] ; 8.10 (s, [1H)] ; 8.00 (s, [1H).] [IR (NUJOL, CM~1)] : 2235.70 [(C--N)] ; 1700.14 [(C=O).] |