참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Formaldehyde | HCID 712 | — |
| 반응물 | Hexamethylenetetramine | HCID 4101 | — |
| 반응물 | 2,3,6-Trimethylphenol | HCID 17016 | — |
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 4-Hydroxy-2,3,5-trimethylbenzaldehyde | HCID 10899021 | 75% |
반응 단계
Instead of hexamethylenetetramine as applied in Example 2A and 2B, formaldehyde and ammonium acetate in acetic acid were used for formylation as illustrated below. A 250 ml three neck round bottom flask equipped with a reflux condenser was charged with 20.4 g (0.15 mol) of 2,3,6-trimethylphenol. 100 ml acetic acid, 3.09 g (0.04 mol) of ammonium acetate and 3.243 g (0.04 mol) of formalin solution were added to it. The reaction mass was heated at 120° C. over a period of 2.5 hrs. The completion of reaction was confirmed by TLC. The reaction mass was poured into 400 ml ice cold water with stirring. The solid was filtered and washed with 2×50 ml process water. The product was dried under vacuum to afford 17 g (75%) of crude 2,3,5-trimethyl-4-hydroxy-benzaldehyde. The purification of crude product with 1% sodium hydroxide solution afforded 13 g (53%) of pure 2,3,5-trimethyl-4-hydroxyl-benzaldehyde.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08846982B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-05837208b17746a08c42c30a85c05bfd |
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| 출처 메모 | uspto-grants-2014_09 |
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