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Limited Quantity | USD 15-60 |
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* Storage: {[proInfo.prStorage]}
CAS No. : | 1513-60-6 | MDL No. : | MFCD00041517 |
Formula : | C7H6F6O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 236.11 | Pubchem ID : | - |
Synonyms : |
|
Signal Word: | Danger | Class: | 3 |
Precautionary Statements: | P210-P233-P240-P241-P242-P243-P261-P264-P270-P271-P280-P301+P312-P302+P352-P303+P361+P353-P304+P340-P312-P322-P330-P363-P370+P378-P403+P235-P501 | UN#: | 1993 |
Hazard Statements: | H225-H302-H312-H332 | Packing Group: | Ⅲ |
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 |
---|---|---|
86% | With ammonia In diethyl ether at 195 - 293℃; | |
85% | With ammonia In diethyl ether 1.) -80 deg C, 40 min, 2.) RT, 3 h; | |
With ammonia |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
92% | In diethyl ether at 0℃; for 0.5h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
91% | In diethyl ether at 0℃; for 0.5h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
74% | In diethyl ether for 2h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
54% | In tetrahydrofuran at -78℃; for 0.5h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
14% | With triethylamine In diethyl ether for 48h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
77% | With triethoxyaluminium hydride In diethyl ether at -78℃; other nucleophiles; | |
77% | With lithium triethoxyaluminum hydride In diethyl ether at -78℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen | ||
With hydrogen |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72% | With hydroxylamine In ethanol at -20℃; for 1h; | |
Ca. 11 g | With hydroxylamine hydrochloride; N-ethyl-N,N-diisopropylamine In ethanol at -20 - 20℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
67% | With sodium hydride In tetrahydrofuran; paraffin at 10℃; for 0.5h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | In diethyl ether at -20℃; for 0.5h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
56% | With sodium hydride In dimethyl sulfoxide 1) 50 deg C, 12 h, 2) 110 deg C, 2 h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
84% | In diethyl ether at -78.1 - 19.9℃; | |
67% | In diethyl ether 1.) -80 deg C, 1.5 h, 2.) RT, 5 h; | |
In toluene |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | With sodium hydride In tetrahydrofuran; paraffin at 10℃; for 0.5h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
50% | With boron trifluoride diethyl etherate at 20℃; for 48h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
99% | Stage #1: 1-methyl-1-nitrosourea With potassium hydroxide In diethyl ether at 0℃; Stage #2: ethyl 4,4,4-trifluoro-3-(trifluoromethyl)crotonate In diethyl ether at 20℃; for 1h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine at 20 - 60℃; for 2h; | 2 17.6 g (0.043 mol) of ethyl 4,4,4-trifluoro-3-trifluoroacetyl-butanoate with a purity of 85.6 % were mixed with 4.10 g (0.041 mol) of triethylamine in a glass flask equipped with a condenser cooled down to 50C. The reaction was started at room temperature, but due to the exothermic nature of the reaction, the temperature increased to 6O0C. After 2 h, the reaction medium was washed first with a NH4Cl saturated water solution (2 x 40 ml) and then with 40 ml of water. The organic phase was separated from the aqueous phase by decantation and dried over MgSO4. Analysis by gas chromatography showed a complete conversion of ethyl 4,4,4-trifluoro-3-trifluoroacetyl-butanoate, with a selectivity of 99 % into ethyl 4,4,4-trifluoro-3-trifluoromethyl crotonate (ETFMC). ETFMC was then distilled under vacuum. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 69 percent / LiAlH4 / diethyl ether / 2.5 h / 20 °C 4.1: 94 percent / Br2; PPh3; pyridine / CH2Cl2 / 12 h / 20 °C | ||
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 69 percent / LiAlH4 / diethyl ether / 2.5 h / 20 °C 4.1: 94 percent / Br2; PPh3; pyridine / CH2Cl2 / 12 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 69 percent / LiAlH4 / diethyl ether / 2.5 h / 20 °C | ||
Multi-step reaction with 3 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 69 percent / LiAlH4 / diethyl ether / 2.5 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating | ||
Multi-step reaction with 3 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 5 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP 5.1: aq. HBr / acetic acid / 20 °C | ||
Multi-step reaction with 5 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP 5.1: aq. HBr / acetic acid / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating | ||
Multi-step reaction with 2 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP | ||
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP | ||
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 6 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP 5.1: aq. HBr / acetic acid / 20 °C 6.1: DCC; DMAP / CH2Cl2 / 12 h / 20 °C | ||
Multi-step reaction with 6 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP 5.1: aq. HBr / acetic acid / 20 °C 6.1: DCC; DMAP / CH2Cl2 / 12 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 5 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 69 percent / LiAlH4 / diethyl ether / 2.5 h / 20 °C 4.1: 94 percent / Br2; PPh3; pyridine / CH2Cl2 / 12 h / 20 °C 5.1: 21 percent / K2CO3 / ethanol / 7 h / Heating | ||
Multi-step reaction with 5 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 69 percent / LiAlH4 / diethyl ether / 2.5 h / 20 °C 4.1: 94 percent / Br2; PPh3; pyridine / CH2Cl2 / 12 h / 20 °C 5.1: 21 percent / K2CO3 / ethanol / 7 h / Heating |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 6 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP 5.1: aq. HBr / acetic acid / 20 °C 6.1: DCC; DMAP / CH2Cl2 / 12 h / 20 °C | ||
Multi-step reaction with 6 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: DCC; DMAP 5.1: aq. HBr / acetic acid / 20 °C 6.1: DCC; DMAP / CH2Cl2 / 12 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: 69 percent / DCC; DMAP / CH2Cl2 / 12 h / 20 °C | ||
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: 69 percent / DCC; DMAP / CH2Cl2 / 12 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 5 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 69 percent / LiAlH4 / diethyl ether / 2.5 h / 20 °C 4.1: 94 percent / Br2; PPh3; pyridine / CH2Cl2 / 12 h / 20 °C 5.1: 52 percent / K2CO3 / ethanol / 7 h / Heating | ||
Multi-step reaction with 5 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 69 percent / LiAlH4 / diethyl ether / 2.5 h / 20 °C 4.1: 94 percent / Br2; PPh3; pyridine / CH2Cl2 / 12 h / 20 °C 5.1: 52 percent / K2CO3 / ethanol / 7 h / Heating |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 99 percent / CCl4 / 7 h / UV-irradiation; heating 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: 79 percent / DCC; DMAP / CH2Cl2 / 12 h / 20 °C | ||
Multi-step reaction with 4 steps 1.1: aq. KOH / diethyl ether / 0 °C 1.2: 99 percent / diethyl ether / 1 h / 20 °C 2.1: 180 °C / Pyrolysis 3.1: 86 percent / NaOH / ethanol; H2O / 3 h / Heating 4.1: 79 percent / DCC; DMAP / CH2Cl2 / 12 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: 86 percent / NH3 / diethyl ether / 195 - 293 °C 2: 91 percent / 6M aq. HCl / 7 h / Heating | ||
Multi-step reaction with 2 steps 1: 85 percent / liguid NH3 / diethyl ether / 1.) -80 deg C, 40 min, 2.) RT, 3 h 2: 80 percent / 6N HCl / 7 h / 90 °C | ||
Multi-step reaction with 2 steps 1: NH3 2: aq. HCl |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: 86 percent / NH3 / diethyl ether / 195 - 293 °C 2: 91 percent / 6M aq. HCl / 7 h / Heating 3: 72 percent / Et3N / dioxane; H2O / Ambient temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: hydrogen / Pd/C 2: lithium aluminum hydride / diethyl ether / 0.5 h / Heating |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1: hydrogen / Pd/C 2: lithium aluminum hydride / diethyl ether / 0.5 h / Heating 3: triphenylphosphine, diethyl azodicarboxylate / tetrahydrofuran / 18 h / Ambient temperature 4: hydrazine monohydrate / ethanol / 1 h / Heating |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: hydrogen / Pd/C 2: lithium aluminum hydride / diethyl ether / 0.5 h / Heating 3: triphenylphosphine, diethyl azodicarboxylate / tetrahydrofuran / 18 h / Ambient temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 6 steps 1: hydrogen / Pd/C 2: lithium aluminum hydride / diethyl ether / 0.5 h / Heating 3: triphenylphosphine, diethyl azodicarboxylate / tetrahydrofuran / 18 h / Ambient temperature 4: hydrazine monohydrate / ethanol / 1 h / Heating 5: 1-<3-(dimethylamino)propyl>-3-ethylcarbodiimide, 4-(dimethylamino)pyridine / CH2Cl2 / 18 h / Ambient temperature 6: lithium hydroxide monohydrate / tetrahydrofuran; methanol / 18 h / Ambient temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 5 steps 1: hydrogen / Pd/C 2: lithium aluminum hydride / diethyl ether / 0.5 h / Heating 3: triphenylphosphine, diethyl azodicarboxylate / tetrahydrofuran / 18 h / Ambient temperature 4: hydrazine monohydrate / ethanol / 1 h / Heating 5: 1-<3-(dimethylamino)propyl>-3-ethylcarbodiimide, 4-(dimethylamino)pyridine / CH2Cl2 / 18 h / Ambient temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 7 steps 1: hydrogen / Pd/C 2: lithium aluminum hydride / diethyl ether / 0.5 h / Heating 3: triphenylphosphine, diethyl azodicarboxylate / tetrahydrofuran / 18 h / Ambient temperature 4: hydrazine monohydrate / ethanol / 1 h / Heating 5: 1-<3-(dimethylamino)propyl>-3-ethylcarbodiimide, 4-(dimethylamino)pyridine / CH2Cl2 / 18 h / Ambient temperature 6: lithium hydroxide monohydrate / tetrahydrofuran; methanol / 18 h / Ambient temperature 7: 1-<(3-dimethylamino)propyl>-3-ethylcarbodiimide, 4-(dimethylamino)pyridine / CH2Cl2 / 18 h / Ambient temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: 35 percent / toluene / 8 h / Heating 2: 91 percent / LiAlH4 / diethyl ether / 0.5 h / 0 °C 3: 78 percent / H2 / 20percent Pd(OH)2/C / ethyl acetate / 5 h / 760 Torr |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: 33 percent / toluene / 8 h / Heating 2: 89 percent / LiAlH4 / diethyl ether / 0.5 h / 0 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: 35 percent / toluene / 8 h / Heating 2: 91 percent / LiAlH4 / diethyl ether / 0.5 h / 0 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: 35 percent / toluene / 8 h / Heating 2: 84 percent / H2 / 20percent Pd(OH)2/C / ethyl acetate / 5 h / 760 Torr |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: 33 percent / toluene / 8 h / Heating 2: 91 percent / H2 / 20percent Pd(OH)2/C / ethyl acetate / 5 h / 1 Torr |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: 85 percent / liguid NH3 / diethyl ether / 1.) -80 deg C, 40 min, 2.) RT, 3 h 2: 80 percent / 6N HCl / 7 h / 90 °C 3: 82 percent / trifluoroacetic acid / 1.) 3 deg C, 1 h, 2.) 20 deg C, 3o min |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: 85 percent / liguid NH3 / diethyl ether / 1.) -80 deg C, 40 min, 2.) RT, 3 h 2: 39 percent / DCC, HOBt / dimethylformamide / 20 h / 60 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: 85 percent / liguid NH3 / diethyl ether / 1.) -80 deg C, 40 min, 2.) RT, 3 h 2: 80 percent / 6N HCl / 7 h / 90 °C 3: 6 percent / p-toluenesulfonic acid monohydrate / benzene / 240 h / Heating |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: 85 percent / liguid NH3 / diethyl ether / 1.) -80 deg C, 40 min, 2.) RT, 3 h 2: 80 percent / 6N HCl / 7 h / 90 °C 3: 1-hydroxybenzotriazole, pyridine / dimethylformamide / 12 h / Ambient temperature |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With SF4 In cyclohexane; water | II 1,1,1,4,4,4-Hexafluoro-2-(trifluoromethyl)butane EXAMPLE II 1,1,1,4,4,4-Hexafluoro-2-(trifluoromethyl)butane A 300 mL autoclave was charged with 21.0 g (0.1 mol) 4,4,4-trifluoro-3-(trifluoromethyl)butyric acid (prepared by hydrogenation and hydrolysis of commercially available ethyl 4,4,4-trifluoro-3-(trifluoromethyl)crotonate), 25 mL cyclohexane, and 38 g (0.35 mol) SF4. The contents were heated to 65°-70° C. for 3 days, vented through a KOH scrubber, and poured into a separatory funnel containing 40 mL water. The aqueous layer was extracted with 2*25 mL portions of cyclohexane, and the combined organic layers distilled. An azeotrope of the desired product and cyclohexane was obtained (bp 41°-2° C.), which contained about 20% cyclohexane. The desired HFC was obtained in 23% yield following extraction with light mineral oil and distillation. A second distillation provided material of 99% purity, bp 43°-44° C. 1H NMR (CDC13): δ 3.25 (m, 1 H) and 2.63 (dq, 2 H); 19 F NMR: 67.3 (3 F) and 69.5 (5F) ppm. %F=70. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 65% 2: 3% | With trimethylsilyl trifluoromethanesulfonate In dichloromethane at 20℃; Inert atmosphere; Overall yield = 68 %; Overall yield = 191 mg; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 53% 2: 8% 3: 7% | In 1,4-dioxane at 135 - 140℃; Sealed tube; Inert atmosphere; |