一二三四区视频,亚洲少妇熟女色,日本久热无码视频网,欧美国产日韩大尺度,亚洲a视频,久久少妇一区二区,日韩999无码视频,刺激久久久久久久,啊啊啊啊不要啊在线

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
010-86108875
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List Propynol ethoxylate
3973-18-0

Propynol ethoxylate synthesis

8synthesis methods
Ethylene glycol

107-21-1

Propargyl bromide

106-96-7

Propynol ethoxylate

3973-18-0

4.2.2. Synthesis of 2-(prop-2-ynyloxy)ethanol (2). Under argon protection, propargyl bromide (2.5 mL, 80% toluene solution, 22.5 mmol) was mixed with ethylene glycol (2.5 mL) and cooled to 0 °C in an ice bath. Powdered NaOH (1.08 g, 45.0 mmol) was slowly added to the reaction system, followed by warming the reaction mixture to 45 °C and stirring for 3 hours. After completion of the reaction, the precipitate was removed by filtration and washed with dichloromethane (23 mL). The filtrates were combined and extracted with dichloromethane (310 mL). The crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=2:1) and after evaporation of the solvent under reduced pressure, 1.34 g (60% yield) of target compound 2 was obtained as a light yellow oil. Thin layer chromatography Rf value 0.25 (Expanding agent: hexane/ethyl acetate=2:1). IR spectrum (neat, cm?1): 1106, 1246, 1729, 2115, 2868, 2935, 3287, 3400. 1H NMR (CDCl?, 250 MHz): δ 2.42 (1H, t, J=2.2 Hz), 2.99 (1H, s), 3.55 (2H, t, J=4.4 Hz), 3.66 (2H, t, J=4.4 Hz), 4.12 (2H, d, J=2.2 Hz).13C NMR (CDCl?, 62.5 MHz): δ 58.1, 61.2, 71.0, 74.6, 79.3.High-resolution mass spectra (ESI): [M+H]? Calculated C?H?O?: 101.0603, measured: 101.0602.

-

Yield:3973-18-0 80%

Reaction Conditions:

Stage #1: ethylene glycolwith sodium hydride in N,N-dimethyl-formamide;mineral oil at 0; for 0.5 h;
Stage #2: propargyl bromide at 0 - 50;

Steps:

1 Step 1:
2-(prop-2-yn-1-yloxy)ethan-1-ol


To a stirred mixture of sodium hydride (60% in mineral oil, 115 mg, 2.8 mmol) in anhydrous N,N-dimethylformamide (20 ml) at 0° C. was added ethane-1,2-diol (3.9 g, 63 mmol) and stirred at 0° C. for 0.5 hour.
To the resulting mixture was added 3-bromoprop-1-yne (5.0 g, 42 mmol) at 0° C. and stirred at 50° C. overnight. TLC showed the reaction was complete.
The reaction mixture was quenched with ice water (20 ml) and partitioned between ethyl acetate (80 ml) and water (100 ml).
The organic layer was collected, and the aqueous layer was extracted with ethyl acetate (50 ml*2).
The combined organic layers were washed with brine (80 ml), dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give a crude residue which was purified by silica gel flash chromatography (eluted with 0-20% ethyl acetate in hexane) to afford 2-(prop-2-yn-1-yloxy)ethanol (3.4 g, yield 80%) as colorless oil.

References:

US2018/125821,2018,A1 Location in patent:Paragraph 0858; 0859

Propynol ethoxylate Related Search:

长兴县| 昌江| 佛山市| 莲花县| 紫金县| 湟中县| 栖霞市| 津市市| 綦江县| 乌鲁木齐县| 南康市| 年辖:市辖区| 六安市| 云霄县| 长沙县| 济源市| 鹰潭市| 丹东市| 报价| 藁城市| 潼关县| 凤山县| 建宁县| 泉州市| 印江| 会东县| 池州市| 太仆寺旗| 吕梁市| 皮山县| 琼海市| 双辽市| 昌都县| 东山县| 阿坝县| 迁安市| 汉寿县| 南开区| 周口市| 伊宁市| 孝义市|