참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-(Methylamino)ethanol | HCID 8016 | — |
| 반응물 | 3-Buten-2-one, 4-(4-hydroxyphenyl)- | HCID 95648 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Sodium Bisulfite | HCID 23665763 | — |
| 생성물 | 4-Phenyl-3-Buten-2-one | HCID 15909 | — |
반응 단계
It should be noted that an initial reaction of 2-methylaminoethanol (1.5 mL) with 4-hydroxybenzylideneacetone (0.68 g) in NaHSO3 (0.78 g) and H2O (1.5 mL) in a sealed vial at 140° C. for 16 hrs did not provide the necessary benzylidene acetone derivative (Scheme 1, compound (b)). Therefore, N-methyl-N-(2-hydroxyethyl)-4-aminobenzaldehyde (Scheme 1, compound (a)) was purchased and used to complete the first step of synthesis instead. When the benzylidene acetone derivative was spotted on a TLC plate the compound glowed fluorescently. The benzylidene acetone derivative reaction mixture was spotted onto preparative TLC plate for purification. Three distinct bands can be observed: a red band at the bottom of the plate, yellow band at the middle, and a faint band at the top were observed. Using mass spectra the inventors determined that the middle yellow band contained the actual benzylidene acetone derivative.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07737183B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-31952cbb8ebb4df5a76aaeb5bfb3ec48 |
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| 출처 메모 | uspto-grants-2010_06 |
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