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A method for the preparation of diazoalkanes

A technology for diazoalkane and alkyl, which is applied in the field of preparing the N-alkyl-N-nitroso compound, can solve problems such as environmental and waste disposal problems, and achieve the effect of high yield

Active Publication Date: 2014-12-10
BAKHU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Also, the use of certain organic solvents may pose environmental and waste disposal issues such that eliminating the need for these solvents would also be advantageous

Method used

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  • A method for the preparation of diazoalkanes
  • A method for the preparation of diazoalkanes
  • A method for the preparation of diazoalkanes

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[0058] Preparation of N-Alkyl-N-nitroso Compounds

[0059]

[0060] The general method of adding an aliphatic amine to a starting material to form an intermediate amine followed by addition of an acid and an alkali metal nitrite to make an N-alkyl-N-nitroso compound is well established in the art. Known. An exemplary method for preparing N-alkyl-N-nitroso compounds according to the present invention is outlined in Scheme 2 above. In the above embodiment, the N-alkyl-N-nitroso compound is N-nitroso-β-methylaminoisobutyl methyl ketone, and the starting material is mesityl oxide. The above-mentioned method can be carried out continuously or in batches.

[0061] One aspect of the invention involves the acidification of amines with tribasic acids. Any tribasic acid can be used, such as phosphoric or citric acid. In another embodiment, the tribasic acid is phosphoric acid. Preferably, the phosphoric acid is between 60% and 80% phosphoric acid in water, most preferably 75% ph...

Embodiment

[0080] Preparation of N-nitroso-β-methylaminoisobutyl methyl ketone

[0081] A 2 L glass reactor was equipped with a 500 mL addition funnel, stirrer, thermometer and cooling bath.

[0082] 1. Charge the reactor with 39.7% aqueous methylamine (230 g) and cool to 10°C.

[0083] 2. When the temperature reached 7°C, the addition of mesityl oxide (300 g) was started. The temperature is controlled between 10°C and 15°C. The total addition time was 57 minutes.

[0084] 3. Warm the clear light orange solution to 22°C over 5 minutes and then stir at this temperature for 60 minutes.

[0085] 4. Cool the solution to 10°C over 5 minutes. 75% phosphoric acid (310.2 g) was added over 60 minutes. Keep the temperature between 15°C and 20°C. During the addition, the mixture became more viscous. The pH at the end of the addition was 6.65.

[0086] 5. Add 30% aqueous sodium nitrite solution (771.3 g) between 10°C and 15°C over 8 minutes.

[0087] 6. Stir the mixture between 20°C and 25°...

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Abstract

The present invention relates to a method of forming diazoalkanes. One aspect of the present invention provides a method for the production of a N-alkyl-N-nitroso compound from a starting material, comprising the use of a tribasic acid to acidify an amine. A second aspect of the present invention provides a method for the production of a diazoalkane, comprising reacting a N-alkyl-N-nitroso compound with a base and a phase transfer catalyst, wherein no organic solvent is used,

Description

technical field [0001] The present invention relates to the preparation of diazoalkane. One aspect provides improved methods for the preparation of diazoalkanes from N-alkyl-N-nitroso compounds. Improved methods for the preparation of said N-alkyl-N-nitroso compounds are also described. Also provided is the use of diazomethane prepared by the method described in the preceding aspect to form tert-butyl (S)-4-chloro-3-oxo-1-phenylbutan-2-ylcarbamate (Boc-CK )Methods. Background technique [0002] Diazoalkanes are important compounds in organic synthesis, and are generally used as intermediates or reactants in reactions such as etherification of NH bonds, OH bonds, or acid bonds, or in the synthesis of heterocyclic compounds. They are also used in addition and insertion reactions under mild conditions. [0003] Diazomethane is a highly reactive gas that has a wide range of uses in chemical synthesis. It is generally used as a methylating agent for various compounds, and in...

Claims

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Application Information

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IPC IPC(8): C07C243/04C07C245/16
CPCC07C245/16C07C243/04C07C241/00C07C2531/02
Inventor 李·普罗克特
Owner BAKHU
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