참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Chloroacetonitrile | HCID 7856 | — |
| 반응물 | p-Chloroacetophenone oxime | HCID 96172 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 반응물 | (alpha-Methyl-4-chlorobenzylidene amino)oxy acetonitrile | HCID 54535538 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Diisopropyl Ether | HCID 7914 | — |
| 생성물 | HCID 54127586 | HCID 54127586 | — |
반응 단계
Of the (α-methyl-4-chlorobenzylidene amino)oxy acetonitrile (melting point 57° C.-58.5° C.) which was obtained by reacting the sodium salt of 4'-chloroacetophenone oxime, with chloroacetonitrile in dimethylformamide, an amount of 11.3 g was dissolved in diisopropyl ether in which 1.94 g of hydrogen chloride and 1.73 g of methanol had also been dissolved. The solution was diluted with 25 ml of diisopropyl ether and subsequently stirred over night. Then the precipitate was drawn off, washed with absolute ether and dried in a vacuum. The resulting hydrochloride of methyl (α-methyl-4-chlorobenzylidene amino)oxy acetimidate melted at 95° C. with decomposition. After this substance had been dissolved in water, the superscribed ester separated out from the solution. It was extracted with ether and distilled in a vacuum. Boiling point at a pressure of 0.1 mm: 130° C.-132° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04196216 |
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| 출처 데이터셋 | uspto-grants-1980_04 |
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| ORD ID | ord-560419011467467dad868d28d2c8f93d |
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| 출처 메모 | uspto-grants-1980_04 |
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