참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3,4,5-Trimethoxybenzaldehyde | HCID 6858 | — |
| 반응물 | 3,4-Dihydro-3-oxo-2H-1,4-benzothiazine-2-acetic acid hydrazide | HCID 3450026 | — |
| 반응물 | 1,2-Dichloroethane ethanol | HCID 22901612 | — |
| 촉매 | Acetic Acid | HCID 176 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 24988117 | HCID 24988117 | — |
반응 단계
In a round-bottom glass flask equipped with a magnetic stir bar (3-Oxo-3,4-dihydro-2H-benzo[1,4]thiazin-2-yl)-acetic acid hydrazide (1 eq. 0.063 mmol; 15 mg) was dissolved in ethanol (3 mL) at room temperature. To this well stirred solution, acetic acid (˜3 drops) and 3,4,5-trimethoxy-benzaldehyde solution (0.063 mmol; 12.4 mg dissolved in 0.5 mL of ethanol) were added, and the reaction mixture was stirred for another 5 hours at ambient temperature and monitored by TLC (typically with 1,2-dichloroethane-ethanol 5:1). The mixture was then concentrated under vacuum using a rotary evaporator. The crude product was diluted with hexanes and triturated. The precipitated solid product was transferred to a glass fiber funnel, the supernatant was removed by vacuum filtration and the solid was washed thoroughly with n-hexane twice to yield: 16 mg (61%) of 1-1.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07786139B2 |
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| 출처 데이터셋 | uspto-grants-2010_08 |
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| ORD ID | ord-446dd4775bbe4a03a3babdfe1b9ddd69 |
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| 출처 메모 | uspto-grants-2010_08 |
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