Water → Diacetyl(methoxyimino)methane

HRID 2306146

反応式

HRID 2306146 の反応式
[C:1](=O)([O-])[O-].[K+].[K+].[CH3:7][C:8](=[O:15])[C:9](=[N:13][OH:14])[C:10](=[O:12])[CH3:11].S(OC)(OC)(=O)=O.O>C(OC)(C)(C)C.CN(C=O)C>[CH3:1][O:14][N:13]=[C:9]([C:10](=[O:12])[CH3:11])[C:8](=[O:15])[CH3:7]

参加物

7

反応物 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 178468373HCID 178468373、化合物

生成物 1

HCID 536122Diacetyl(methoxyimino)methane収率 89%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 15413tert-Butyl methyl ether溶媒

反応条件

温度
-5 °C

実験手順

In a 20 l vessel, 4.5 kg (32.6 mol) of potassium carbonate were suspended in 3.2 l of methyl tert-butyl ether and a liter of DMF. With stirring, the mixture was cooled to from 0 to −10° C. A solution of 4128 g (32 mol) of pentane-2,3,4-trione 3-oxime, 2 l of DMF and 4032 g (32 mol) of dimethyl sulfate was then metered in at an internal temperature of <25° C. over a period of 2 hours. The mixture was stirred at room temperature for another 3.5 hours. A further 20 l of water were then added, the upper, organic phase was removed, the aqueous phase was washed with 2 l of methyl tert-butyl ether, the combined organic phases were washed with 1 l of 5% strength hydrochloric acid and the solvent was distilled off. This gave 4214 g of the title compound in a purity of 96.6% (GC area percent), corresponding to a yield of 89%.

後処理

  1. stirringThe mixture was stirred at room temperature for another 3.5 hours
  2. customthe upper, organic phase was removed
  3. washthe aqueous phase was washed with 2 l of methyl tert-butyl ether
  4. washthe combined organic phases were washed with 1 l of 5% strength hydrochloric acid
  5. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-c7a17002782a4f7aa124f709e0c628b1
出典データセット
uspto-grants-2002_08
特許番号
US06441236B1

関連ノート

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