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CAS RN: 540-80-7 | 產(chǎn)品編碼: N0357
tert-Butyl Nitrite
純度/分析方法: >90.0%(GC)
- 亞硝酸叔丁酯
- Nitrous Acid tert-Butyl Ester
規(guī)格 | 單價(jià) | 上海 | 天津 | 日本* | 數(shù)量 | 庫(kù)存詳情 |
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25ML |
¥460.00
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32 | 從上海倉(cāng)庫(kù)發(fā)貨 | ≥60 |
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|
100ML |
¥1,150.00
|
3 | 從上海倉(cāng)庫(kù)發(fā)貨 | 請(qǐng)聯(lián)系我們 |
|
|
250ML |
¥2,200.00
|
3 | 從上海倉(cāng)庫(kù)發(fā)貨 | ≥40 |
|
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Appearance | Colorless to Yellow to Orange clear liquid |
Purity(GC) | min. 90.0 % |
沸點(diǎn) | 63 °C |
閃點(diǎn) | -13 °C |
比重 | 0.87 |
折射率 | 1.37 |
水溶性 | 微溶, 與水接觸發(fā)生分解 |
溶解性(可與之混溶) | 醇 |
象形圖 | |
信號(hào)詞 | 危險(xiǎn) |
危險(xiǎn)性說(shuō)明 | H302 + H332 : 吞咽或吸入有害。 H370 : 會(huì)損害器官。 H225 : 高度易燃液體和蒸氣。 |
防范說(shuō)明 | P501 : 將內(nèi)裝物/容器送到批準(zhǔn)的廢物處理廠處理。 P260 : 不要吸入粉塵/ 煙/ 氣體/ 煙霧/ 蒸氣/ 噴霧。 P270 : 使用本產(chǎn)品時(shí)不要進(jìn)食、飲水或吸煙。 P240 : 容器和裝載設(shè)備接地/等勢(shì)聯(lián)接。 P210 : 遠(yuǎn)離熱源/火花/明火/熱表面。禁止吸煙。 P233 : 保持容器密閉。 P243 : 采取防止靜電放電的措施。 P241 : 使用防爆的電氣/通風(fēng)/照明設(shè)備。 P242 : 只能使用不產(chǎn)生火花的工具。 P271 : 只能在室外或通風(fēng)良好之處使用。 P264 : 作業(yè)后徹底清洗皮膚。 P280 : 戴防護(hù)手套/戴防護(hù)眼罩/戴防護(hù)面具。 P370 + P378 : 火災(zāi)時(shí):使用干砂、干粉或抗醇泡沫滅火。 P308+P311 : 如接觸到或有疑慮:呼叫急救中心/醫(yī)生。 P303 + P361 + P353 : 如皮膚(或頭發(fā))沾染:立即脫掉所有沾污的衣物。用水清洗皮膚/淋浴。 P301 + P312 + P330 : 如誤吞咽:如感覺(jué)不適,呼叫急救中心/醫(yī)生。漱口。 P304 + P340 + P312 : 如誤吸入:將人轉(zhuǎn)移到空氣新鮮處,保持呼吸舒適體位。如感覺(jué)不適,呼叫急救中心/醫(yī)生。 P403 + P235 : 存放在通風(fēng)良好的地方。保持低溫。 P405 : 存放處須加鎖。 |
RTECS# | RA0802000 |
新化學(xué)物質(zhì)備案回執(zhí)號(hào) | B1A232215097 |
UN編號(hào) | UN2351 |
類(lèi)別 | 3 |
包裝類(lèi)別 | II |
監(jiān)管條件代碼(*) |
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Used Chemicals
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Procedure
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To a solution of p-anisidine (123 mg, 1.0 mmol), p-TsOH-H2O (190 mg, 1.0 mmol, 1.0 eq.), KI (415 mg, 2.5 mmol, 2.5 eq.) in acetonitrile (5 mL) was added dropwise tBuONO (0.30 mL, 2.5 mmol, 2.5 eq.) at 0 °C and the mixture was stirred at same temperature for 30 min. Then the reaction mixture was heated 60 °C and stirred for 4 h. After quenching with water (15 mL), it was extracted with ethyl acetate (15 mL x 3) and the organic layer was washed with 2 mol/L HCl aq. (15 mL), sat. NaHCO3 aq. (15 mL), brine (15 mL), dried over sodium sulfate and filtered. The solvent was removed under reduced pressure and the residue was purified by column chromatography (on silica gel, ethyl acetate:hexane = 1:4) to give 4-iodeanisole as a red solid (202 mg, 86% yield).
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Experimenter’s Comments
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The reaction mixture was monitored by UPLC.
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Analytical Data
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4-iodeanisole
1H NMR (400 MHz, CDCl3); δ 7.56 (d, J = 8.0 Hz, 2H), 6.68 (d, J = 8.0 Hz, 2H), 3.78 (s, 3H).
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Lead Reference
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- A New, One-Step, Effective Protocol for the Iodination of Aromatic and Heterocyclic Compounds via Aprotic Diazotization of Amines
Reference
- Benzyne Click Chemistry with in Situ Generated Aromatic Azides
1. Chlorination:1)
To a mixture of copper(II)chloride (24.35 g, 181.2 mmol), dry acetonitrile (200 mL) and tert-butyl nitrite (25.7 mL, 226.5 mmol), a solution of 4-bromo-2-chloro-5-fluoroaniline (33.9 g, 151 mmol) in dry acetonitrile (200 mL) is added at 60 ℃ under nitrogen. The mixture is stirred for 30 min at 60 ℃, followed by cooling to room temperature and addition of 2M HCl (400 mL). The phases are separated, and the water phase is extracted with diethyl ether (150 mL). The combined organic phases are washed with water and dried over MgSO4. The organic phase is concentrated on the rotary evaporator and is distilled at 150 ℃/ 20 mbar, yielding colourless oil (30 g, 111 mmol, 72% yield, 90% purity).
Anhydrous copper(II) bromide (6.8 g, 30.5 mmol), tert-butyl nitrite (4.3 mL, 36 mmol), and anhydrous acetonitrile (150 mL) are added to a three-neck round-bottom flask, and the mixture is heated to 65 ℃. 2,7-Diamino-9,10-anthraquinone (2.9 g, 12 mmol) is added slowly over a period of 5 min to the reaction mixture. Nitrogen is evolving during the reaction. After nitrogen evolution have subsided, the reaction mixture is cooled to room temperature and poured into an aqueous 20% HCl solution (100 mL). The crude solid product is collected, washed with ether, and chromatographed on a silica gel column (hexane : CH2Cl2 = 1: 1) to afford the desired product (2.6 g, Y.60%) as a yellow solid.
References
- 1)Synthesis of Dioxin-like Monofluorinated PCBs: for the Use as Internal Standards for PCB Analysis.
- 2)Arylethynyl Substituted 9,10-Anthraquinones: Tunable Stokes Shifts by Substitution and Solvent Polarity.
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