참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | Acryloyl chloride | HCID 13140 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Aminoacetaldehyde dimethyl acetal | HCID 89728 | — |
| 촉매 | 2,2,6,6-tetramethyl-4-hydroxypiperidine-N-oxide | HCID 11607999 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | N-(2,2-Dimethoxyethyl)-2-propenamide | HCID 9898899 | 81.7% |
반응 단계
40 g (1.0 mol) of sodium hydroxide are dissolved in 100 g of water and 200 g of ice in a 1 litre reactor fitted with stirring and cooling means. The sodium hydroxide solution is cooled to 10° C., and 105.1 g (1.0 mol) of aminoacetaldehyde dimethyl acetal and 10 mg of the inhibitor 4-hydroxy-2,2,6,6-tetrarnethylpiperidine 1-oxide are added. 99.5 g (1.1 mol) of acryloyl chloride are slowly added to this solution at 10° C. over the course of 2 hours. The pH drops slowly and is finally set to pH=7. Amine is no longer present according to GC. The reaction mixture is saturated with sodium chloride and extracted three times with 200 ml of tert-butyl methyl ether. The organic phase is dried, filtered and evaporated on a rotary evaporator. The resultant oil is extracted three times with petroleum ether and subsequently re-dried on a rotary evaporator, giving 130 g of acrylamidoacetaldehyde dimethyl acetal (81% of theory) as an oil. The product is 99% pure according to GC. ##STR29##
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05932674 |
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| 출처 데이터셋 | uspto-grants-1999_08 |
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| ORD ID | ord-9629e37cf3c240cc86c1b4dfe34b6af6 |
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| 출처 메모 | uspto-grants-1999_08 |
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