참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Hexamethylenetetramine | HCID 4101 | — |
| 반응물 | 4-Chloro-3-methylbut-2-en-1-yl acetate | HCID 53400932 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-Formylbut-2-enyl acetate | HCID 84699 | 69% |
반응 단계
Crude 4-acetoxy-2-methyl-1-chloro-2-butene (194 g, Purity: 83.8%, 1 mol) was added to hexamethylenetetramine (168 g, 1.2 mol)/water (1 liter), and the mixture was stirred at 35° C. for 4 hours and then separated into aqueous and organic layers. 1,2-Dichloroethane (1 liter) was added to the aqueous layer, the mixture was subjected to reaction at 72° C. for 6 hours while adjusting the pH with 1N sulfuric acid. The 1,2-dichloroethane layer was separated, 1,2-dichloroethane (1 liter) was added, and the reaction was carried out again. The 1,2-dichloroethane layers were combined and concentrated. The residue was distilled under reduced pressure to give 4-acetoxy-2-methyl-2-buten-1-al (98 g, 69%). bp.0.2-0.3 : 58°-66° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05424478 |
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| 출처 데이터셋 | uspto-grants-1995_06 |
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| ORD ID | ord-aab0f7af60384a74ae6c7680925421cb |
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| 출처 메모 | uspto-grants-1995_06 |
|---|