917-92-0Relevant articles and documents
Hargrove,R.J.,Stang,J.S.
, p. 581 - 582 (1974)
Kocienski
, p. 3285 (1974)
Preparation method of 3, 3-dimethyl-1-butyne
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Paragraph 0028-0031; 0034-0043, (2021/04/17)
The invention discloses a preparation method of 3, 3-dimethyl-1-butyne, which comprises the following steps: by using tert-butyl alcohol and acetylene which are simple, readily available and cheap as initial raw materials and using transition metal salt which is readily available on the market as a catalyst, directly reacting in the presence of acid to obtain a product, and carrying out simple distillation separation to obtain a high-purity product. The method is simple and convenient to operate, less in environmental pollution, good in product quality, high in yield, low in cost and more suitable for industrial production.
Synthesis method of terbinafine medical intermediate tert-butyl acetylene
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Paragraph 0015; 0016, (2017/03/14)
A synthesis method of terbinafine medical intermediate tert-butyl acetylene includes the following steps of adding 310 ml of potassium bisulfite solution and 300 ml of potassium bisulfite to a reaction vessel provided with a stirrer, a thermometer, a dropping funnel and a condenser, raising the temperature of the solution to 90-95 DEG C, controlling the stirring speed at 150-170 rpm, dropwise adding 0.73 mol of 1,1-diamido-3,3-dimethylbutane, controlling the dropwise adding time at 3-5 hours, adding 0.81-0.84 mol of hypochloric acid phenyl ester, conducting reaction for 90-120 min, raising the temperature of the solution to 110-115 DEG C, continuing to conduct reaction for 3-5 hours, lowering the temperature of the solution to 10-15 DEG C, separating out solid, conducting filtering, saline solution washing, acetonitrile washing and pressure reduction distillation, collecting fraction of 100-108 DEG C, and conducting recrystallization in cyclohexane to obtain crystal tert-butyl acetylene.
Substituent effects on the photorearrangements of unsymmetrically substituted diazinobarrelenes
Hsieh, Hsing-Pang,Chen, Ann-Cheng,Villarante, Nelson R.,Chuang, Gary J.,Liao, Chun-Chen
, p. 1165 - 1178 (2013/03/14)
A series of diazinobarrelenes 8-15 engendered with alkyl functionalities at the barrelene skeleton were irradiated with 350 nm light under direct and acetone-sensitized reaction conditions. Under these conditions, all the barrelenes except barrelene 14 afforded semibullvalenes with varying degrees of regioselectivity and product distribution. Dicyanopyrazinobarrelenes 8-10 which furnished semibullvalenes 32-41via the aryl-vinyl initial bridging route were strongly controlled by the nitrile functionalities installed at the aromatic sites. Benzoquinoxalinobarrelenes 11-13 which afforded semibullvalenes 42-49, preferentially underwent photorearrangement via vinyl-vinyl bridging even if the compounds were excited at a wavelength where the quinoxaline moiety absorbed most of the light. Zimmerman's bridging hypothesis and the possibility for quinoxalines to undergo intramolecular triplet energy transfer could reasonably account for the observed regioselectivity. Barrelene 14 was insensitive to photorearrangement whereas benzo[f,h]quinoxalinobarrelene 15 preferentially underwent ADPM rearrangement affording semibullvalenes 50-52. Electronic and steric factors of alkyl substituents overwhelmingly controlled the product forming steps whereas localization and minimization of triplet energies greatly influenced the initial bridging interaction. The Royal Society of Chemistry 2013.