1-甲氧基-1-烷硫基丙烷的合成

甲氧基烷硫基丙烷;丙缩醛;硫醇;1-甲氧基-1-烷硫基丙烷的合成     

1-甲基-1-乙氧基-1-烷硫基甲烷类化合物的合成研究

本文以乙缩醛和烷基硫醇为原料,在30－35℃于四氯化碳中反应20min左右,分别合成1－甲基－1－乙氧基－1－烷硫基甲烷,经红外光谱,质谱以及核磁共振谱检测,确证了产物结构。     

1-烷基-1''-乙酰基二茂铁的合成

用新方法合成了1-烷基-1'-乙酰基二茂铁,该法与传统方法相比易于得到单一产物.通过7种1-烷基二茂铁甲酸与三氯化磷作用形成酰氯,再与乙酰乙酸乙酯的钠盐进行反应,皂化脱羧得到1-烷基-1'-乙酰基二茂铁化合物,用元素分析、红外光谱、核磁共振氢谱确定了化合物的结构.     

1-烷基-1'-乙酰基二茂铁的合成

用新方法合成了1-烷基-1'-乙酰基二茂铁, 该法与传统方法相比易于得到单一产物. 通过7种1-烷基二茂铁甲酸与三氯化磷作用形成酰氯, 再与乙酰乙酸乙酯的钠盐进行反应, 皂化脱羧得到1-烷基-1'-乙酰基二茂铁化合物, 用元素分析、红外光谱、核磁共振氢谱确定了化合物的结构.     

Synthesis of 1-adamantyloxyalkanols

Russian Journal of Organic Chemistry -     

Synthesis of 1-azapyrene

The environmental contaminants 1-azapyrene 15 , 2-azapyrene 13 and several other azapyrene derivatives were synthesized from a common intermediate, 2,2a,3,4-tetrahydrocyclopenta[cd]phenalen-1-one oxime 6 . The synthesis of 1-azapyrene 15 completes the series of azapyrenes.     

Synthesis of 1-hetarylethylphosphonates

Previously unknown potentially biologically active diethyl 1-(pyridin-3-yl)-, 1-(quinolin-3-yl)-, and 1-(quinolin-6-yl)ethylphosphonates were synthesized by palladium-catalyzed reduction of the corresponding α,β-unsaturated precursors with ammonium formate. The reduction of diethyl 1-(quinolin-6-yl)ethenylphosphonate was accompanied by formation of diethyl 1-(1,2,3,4-tetrahydroquinolin-6-yl)ethylphosphonate as by-product.     

Synthesis of 1-cyanocarboranes

Conclusions A method was developed for the preparation of the 1-cyano-o-and m-carboranes by the reaction of either the C-lithium or C-bromomagnesium o- and m-carboranes with the aromatic esters of cyanic acid.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No.1, pp.217–218, January, 1976.     

Synthesis of 1-TRiacontanol

Several studies describing the synthesis of 1-triacontanol have appeared¹ following the report² that application of 1-triacontanol (1), an active constituent of alfalfa (Medicago sativa L.), increased the yields of tomatoes, cucumber, lettuce, rice, corn and several other crop species. We detail here a convenient synthesis of 1-triacontanol, and the salient feature of this synthesis is that these reactions are inexpensive, simple and amenable to multigram synthesis.     

Synthesis of 1-phosphaadamantane

The annelation reaction between 1,2,3,6-tetrahydro-1-phenyl-4-(1-pyrrolidinyl)phosphorin 1-oxide (4) and ethyl 2-bromomethyl-3-bromopropanoate (5) yielded a mixture of two stereoisomers of the 3-phosphabicyclo[3.3.1]nonane derivative 6. The keto function of 6 was reductively removed to furnish 8 which with LiAlH₄ was reduced to 9. Treatment of 9 with trichlorosilane gave the 1-phenylphosphoniaadamantane 11. The phenyl group of 11 was cleaved with sodium to give the title compound 1, or with NaOH to give the oxide 12 of 1. With benzyl bromide, 1 was quaternized to 13.     

Synthesis of 1-Hydroxyoxindoles

A convenient synthesis of various substituted 1-hydroxyoxindoles is described.     

Synthesis of 1-Trimethylsilyladamantane

The title compound was obtained from 1,3-dichloro-adamantane and some silylating reagents with Na-HMPA.     

Synthesis of 1-arylcyclopropylphosphonates

A simple method for the synthesis of 1-arylcyclopropylphosphonates was proposed. The method involves treatment of 1-arylethenylphosphonic acids or their esters with diazomethane followed by thermolysis of intermediate 3-aryl-4,5-dihydro-3H-pyrazol-3-ylphosphonates. Dedicated to Academician G. A. Abakumov on the occasion of his 70th birthday. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1820–1826, September, 2007.     

Synthesis of 1-formyldipyrromethanes

1-Formyldipyrromethanes are versatile precursors to porphyrins and chlorins. Two methods of synthesis of 1-formyldipyrromethanes have been investigated: (1) Vilsmeier formylation followed by selective removal of the unwanted 1,9-diformyldipyrromethane by dialkyltin complexation and (2) reaction with mesitylmagnesium bromide (MesMgBr) followed by formylation with phenyl formate. The two approaches are complementary (acidic versus basic conditions; statistical versus selective formylation). The latter was found to be more efficient for the preparation of 1-formyldipyrromethanes.