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[ CAS No. 1355636-63-3 ] {[proInfo.proName]}

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Chemical Structure| 1355636-63-3
Chemical Structure| 1355636-63-3
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Product Details of [ 1355636-63-3 ]

CAS No. :1355636-63-3 MDL No. :MFCD28009838
Formula : C7H4Br2ClF Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 302.37 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 1355636-63-3 ]

* 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.

  • Downstream synthetic route of [ 1355636-63-3 ]

[ 1355636-63-3 ] Synthesis Path-Downstream   1~5

  • 1
  • [ 93765-83-4 ]
  • [ 1355636-63-3 ]
YieldReaction ConditionsOperation in experiment
56% With N-Bromosuccinimide; 2,2'-azobis(isobutyronitrile); In tetrachloromethane; for 3.0h;Reflux; Inert atmosphere; The mixture of l-bromo-5-chloro-2-fluoro-4-methyl-benzene (10.0 g, 44.75 mmol, 1.0 eq), NBS (7.9 g, 44.75 mmol, 1.0 eq) and AIBN (736 mg, 4.48 mmol, 0.1 eq) in CCL (250 mL) was heated to reflux and kept stirring for 3 h under N2. The mixture was concentrated. The residue was purified by column chromatography (PE-PE/EA = 30/1, v/v) to give l -bromo-4-bromomethyl-5-chloro-2-fluoro-benzene (7.5 g, 56%) as a yellow oil.
47% With N-Bromosuccinimide; 2,2'-azobis(isobutyronitrile); In tetrachloromethane; at 90℃; for 16.0h; A mixture of <strong>[93765-83-4]1-bromo-5-chloro-2-fluoro-4-methylbenzene</strong> (500 mg, 2.3 mmol), N-bromosuccinimide (481 mg, 2.7 mmol) and azobisisobutyronitrile (38 mg, 0.23 mmol) in CCl4 (10 mL) was stirred at 90 C for 16 h. The mixture was diluted with DCM (20 ml) and water (20 ml). The organic layer was separated, dried over Na2S04, filtered and evaporated to get crude product. The residue was purified by silica column chromatography (eluting with petroleum ether/ethyl acetate = 50/1) to give 1-bromo-4-(bromomethyl)-5-chloro-2-fluorobenzene as a solid (324 mg, 47%).
With N-Bromosuccinimide; dibenzoyl peroxide; In tetrachloromethane; at 85℃; for 18.5h;Inert atmosphere; Preparation 21 -Bromo-4-(bromonnethyl)-5-chloro-2-fluorobenzeneA s o l u t i o n o f <strong>[93765-83-4]4-bromo-2-chloro-5-fluorotoluene</strong> (997 mg, 4.46 mmol), N- bromosuccinimide (837 mg, 4.70 mmol) and benzoyl peroxide (35 mg, 0.14 mmol) in carbon tetrachloride (20 mL) was heated to reflux at 85C for 18.5 hours under nitrogen. The reaction mixture was concentrated in vacuo to afford a cream solid residue. The residue was suspended in heptane (40 mL), filtered and the filtrate then concentrated in vacuo to afford the title compound a clear oil (1 .35 g, 100 %). The compound was used without further purification in the next step.1H NMR (400 MHz, CDCI3): delta 4.50 (s, 2H), 7.24 (d, 1 H), 7.62 (d, 1 H).
With N-Bromosuccinimide; 2-(4-biphenylyl)-5-phenyloxazole; In tetrachloromethane; at 80℃; for 15.0h;Inert atmosphere; To a solution of l-bromo-5-chloro-2-fluoro-4-methylbenzene (14 g, 63.06 mmol) in CCLt (120 mL) were added NBS ( 12.2 g, 69.37 mmol) and BPO (762 mg, 3.15 mmol) under nitrogen. The reaction mixture was stirred at 80C for 15 h. The mixture was cooled, washed with water, extracted with DCM (2 x 50 mL). The combined organic layers were washed with brine (1 x 100 mL), dried over Na2SC>4 and concentrated to give 199 (16 g, crude) which was used for the next step without further purification. LCMS m z 303.4 (M+l )+.

  • 2
  • [ 177480-81-8 ]
  • [ 1355636-63-3 ]
  • 3
  • [ 1355636-63-3 ]
  • [ 1356476-27-1 ]
  • [ 2304652-26-2 ]
YieldReaction ConditionsOperation in experiment
78% Stage #1: 2-(hydroxymethyl)-7-azaspiro[3.5]decane-7-carboxylic acid tert-butyl ester With sodium hydride In N,N-dimethyl-formamide at 0℃; for 0.5h; Stage #2: 1-bromo-4-(bromomethyl)-5-chloro-2-fluorobenzene In N,N-dimethyl-formamide at 0℃; for 0.5h; 1.3 2-(((4-Bromo-2-chloro-5-fluorobenzyl)oxy)methyl)-7-azaspiro[3.5]decane-7-carboxylic acid tert-butyl ester 2-(Light methyl)-7-azaspiro[3.5]decane-7-carboxylic acid tert-butyl ester Id (5.0 g, 20 mmol) was dissolved in 20 mL of N,N-dimethylformamide at 0 °C. Sodium hydride (1.6 g, 40 mmo 1) was slowly added and stirred at 0 ° C for 0.5 hour. 1-Bromo-4-(bromomethyl)-5-chloro-2-fluorobenzene 1 c (6.0 g, 20 mmol) was dissolved in 2 mL of N,N-dimethylformamide and slowly added dropwise at 0 °C.The reaction solution was reacted at 0 ° C for 0.5 hour. The reaction mixture was quenched with water (20 mL), EtOAc (EtOAc (EtOAc) Concentration by pressure, the residue obtained was purified by silica gel column chromatography (eluent: A system) to give 2-(((4-(bromo-2-chloro-5-fluorobenzyl)oxy)methyl)- 7-Azaspiro[3.5]decane-7-carboxylic acid tert-butyl ester 1 e (7.4 g, yellow solid), yield: 78%.
  • 4
  • [ 614730-97-1 ]
  • [ 1355636-63-3 ]
  • 4-(((4-bromo-2-chloro-5-fluorobenzyl)oxy)methyl)-4-fluoropiperidine-1-carboxylic acid tert-butyl ester [ No CAS ]
YieldReaction ConditionsOperation in experiment
85% 4-Fluoro-4-(hydroxymethyl)piperidine-1-carboxylic acid tert-butyl ester 13b (4.7 g, 10.4 mmol) was dissolved in 20 mL of N,N-dimethylformamide at 0 C, slowly adding sodium hydride (832 mg, 20.8 mmol), stirred at 0 C for 0.5 h. 1-Bromo-4-(bromomethyl)-5-chloro-2-fluorobenzene 1c (3.1 g, 10.4 mmol) was dissolved in 2 mL of N,N-dimethylformamide and slowly added dropwise at 0 C.In the reaction solution, the reaction was carried out at 0 C for 0.5 hour. Quench the reaction by adding 20 mL of water to the reaction solution, and extract with ethyl acetate (50 mL×3)The organic phase was combined, washed with a saturated sodium chloride solution (50 mL), and the aqueous layer was evaporated.The residue was purified by silica gel column chromatography (eluent: A) to give 4-(((4-(4-bromo-2-chloro-5-fluorobenzyl)Tert-butyl tert-butyl ester 13c (4.0 g, yellow solid), yield: 85%.
  • 5
  • [ 1126650-66-5 ]
  • [ 1355636-63-3 ]
  • 3-(((4-bromo-2-chloro-5-fluorobenzyl)oxy)methyl)-3-fluoroazetidine-1-carboxylic acid tert-butyl ester [ No CAS ]
YieldReaction ConditionsOperation in experiment
48% Stage #1: 3-fluoro-3-hydroxymethylazetidine-1-carboxylic acid tert-butyl ester With sodium hydride In N,N-dimethyl-formamide at 0℃; for 0.25h; Stage #2: 1-bromo-4-(bromomethyl)-5-chloro-2-fluorobenzene In N,N-dimethyl-formamide at 0℃; for 0.5h; 25.3 3-((4-Bromo-2-chloro-5-fluorobenzyl)oxy)methyl)-3-fluoroazetidine-1-carboxylic acid tert-butyl ester Dissolving 3-fluoro-3-(hydroxymethyl)azetidin-1-carboxylic acid tert-butyl ester 25c (8.9 g, 43.4 mmol) at 0 °CSodium hydride (3.47 g, 86.8 mmol) was slowly added to 70 mL of N,N-dimethylformamide and stirred at 0 ° C for 15 min. Will be 1-Bromo-4-(bromomethyl)-5-chloro-2-fluorobenzene 1c (13.0 g, 43.4 mmol) was dissolved in 60 mL of N,N-dimethylformamide at 0 ° CThe mixture was slowly added dropwise to the above reaction solution, and reacted at 0 ° C for 0.5 hour. The reaction solution was quenched by adding 40 mL of water to ethyl acetate.(100mL × 3) extraction, the organic phase was combined, washed with saturated sodium chloride solution (100mL), the aqueous layer was separated, the organic phase was anhydrous sulfurThe sodium salt was dried, filtered, and concentrated under reduced pressure.((4-Bromo-2-chloro-5-fluorobenzyl)oxy)methyl)-3-fluoroazetidine-1-carboxylic acid tert-butyl ester 25d (8.9g, light yellow oilShape), yield: 48%. MS m/z (ESI): 369.7 [M-55]
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