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[ CAS No. 68737-65-5 ] {[proInfo.proName]}

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Chemical Structure| 68737-65-5
Chemical Structure| 68737-65-5
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Product Details of [ 68737-65-5 ]

CAS No. :68737-65-5 MDL No. :MFCD00671527
Formula : C8H18N2 Boiling Point : -
Linear Structure Formula :- InChI Key :JRHPOFJADXHYBR-HTQZYQBOSA-N
M.W : 142.24 Pubchem ID :2733821
Synonyms :

Safety of [ 68737-65-5 ]

Signal Word:Danger Class:8
Precautionary Statements:P280-P305+P351+P338-P310 UN#:3259
Hazard Statements:H302-H314 Packing Group:Ⅲ
GHS Pictogram:

Application In Synthesis of [ 68737-65-5 ]

* 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 [ 68737-65-5 ]

[ 68737-65-5 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 7343-33-1 ]
  • potassium phosphate [ No CAS ]
  • [ 68737-65-5 ]
  • [ 103962-05-6 ]
  • [ 1417885-96-1 ]
YieldReaction ConditionsOperation in experiment
With hydrogenchloride; In N,N-dimethyl-formamide; Example 5 Preparation of 3-bromo-1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazole A dry round bottom flask was charged with potassium phosphate (K3PO4, 7.74 g, 36.5 mmol), CuI (0.165 g, 0.868 mmol), and <strong>[7343-33-1]3-bromo-1H-1,2,4-triazole</strong> (2.83 g, 19.10 mmol). The flask was evacuated/backfilled with N2 (3*). DMF (34.7 ml) was added, followed by trans-(1R,2R)-N,N'-bismethyl-1,2-cyclohexane diamine (0.274 ml, 1.736 mmol) and 1-iodo-4-(trifluoromethoxy)benzene (5 g, 17.36 mmol). The solution was heated to 110° C. After 48 h, the reaction mixture was cooled to RT, diluted with EtOAc and filtered through Celite?. The filtrate was washed with water (100 mL) containing HCl (1 M, 10 mL). The organics were separated, and the aqueous phase was further extracted with EtOAc (3*). The organics were combined, dried, and concentrated in vacuo. Purification via flash column chromatography EtOAc/hexanes yielded the title compound as a tan solid (1.86 g, 34percent): 1H NMR (400 MHz, CDCl3) delta 8.44 (s, 1H), 7.70 (d, J=8.9 Hz, 2H), 7.38 (d, J=8.5 Hz, 2H); 19F NMR (376 MHz, CDCl3) delta-58.04; EIMS m/z 307 ([M]+).
With hydrogenchloride; In N,N-dimethyl-formamide; Example 5 Preparation of 3-bromo-1-(4-(trifluoromethoxy)Phenyl)-1H-1,2,4-triazole A dry round bottom flask was charged with potassium phosphate (K3PO4, 7.74 g, 36.5 mmol), CuI (0.165 g, 0.868 mmol), and <strong>[7343-33-1]3-bromo-1H-1,2,4-triazole</strong> (2.83 g, 19.10 mmol). The flask was evacuated/backfilled with N2 (3*). DMF (34.7 mL) was added, followed by trans-(1R,2R)-N,N'-bismethyl-1,2-cyclohexane diamine (0.274 mL, 1.736 mmol) and 1-iodo-4-(trifluoromethoxy)benzene (5 g, 17.36 mmol). The solution was heated to 110° C. After 48 h, the reaction mixture was cooled to RT, diluted with EtOAc and filtered through Celite?. The filtrate was washed with water (100 mL) containing HCl (1 M, 10 mL). The organics were separated, and the aqueous phase was further extracted with EtOAc (3*). The organics were combined, dried with sodium sulfate, and concentrated in vacuo. Purification via flash column chromatography (EtOAc/hexanes) yielded the title compound as a tan solid (1.86 g, 34percent): 1H NMR (400 MHz, CDCl3) delta 8.44 (s, 1H), 7.70 (d, J=8.9 Hz, 2H), 7.38 (d, J=8.5 Hz, 2H); 19F NMR (376 MHz, CDCl3) delta-58.04; EIMS m/z 307 ([M]+).
  • 2
  • [ 893566-75-1 ]
  • [ 68737-65-5 ]
  • tert-butyl 8-iodo-3,4-dihydroisoquinoline-2(1H)-carboxylate [ No CAS ]
YieldReaction ConditionsOperation in experiment
94.8% With copper(l) iodide; sodium iodide; In 1,4-dioxane; at 110℃; for 48h;Inert atmosphere; Sealed tube; Large scale; With N2 in dioxane (20 mL)8-bromo-3,4-dihydroisoquinoline-2(1H)-carboxylic acid tert-butyl ester(R-1) (1100 mg, 3.52 mmol), NaI (4.76 g, 31.8 mmol),CuI (402 mg, 2.12 mmol) and trans-N,N-dimethylcyclohexaneThe mixture of (602 mg, 4.22 mmol) was purified for 10 minutes.The resulting yellow suspension was stirred in a sealed tube at 110° C. for 48 hours. The reaction was diluted with petroleum ether (50 mL) and filtered.The filtrate was concentrated in vacuo and the residue was purified by tannin chromatography for petroleum etherThe EtOAC in (from 0 to 20percent) was purified by stripping to provide R-2 (1200 mg, 94.8percent) as a pale yellow gum.
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