Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,3-Cyclohexanedione, 2-acetyl-5,5-dimethyl- → HCID 178464540, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,3-Cyclohexanedione, 2-acetyl-5,5-dimethyl- | HCID 519448 | — |
| 반응물 | (3R,4R,5S,6R)-3-amino-6-(hydroxymethyl)oxane-2,4,5-triol hydrochloride | HCID 2723635 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 178464540 | HCID 178464540 | 188.5% |
반응 단계
Glucosamine hydrochloride (50 g, 231 mmol) was suspended in anhydrous methanol (500 mL), then 2-acetyl-dimedone sodium salt (47.3 g, 231 mmol) was added. The reaction mixture was stirred at room temperature for 10 minutes, then 2-acetyl-dimedone (21.1 g, 115.9 mmol) was added. The reaction mixture was stirred under reflux for 2.5 hours and monitored by tlc. At the completion of the reaction (TLC: MeCN—H20, 10:2), the reaction mixture was cooled to room temperature and filtered. The filtrate was evaporated and the resulting solid residue was washed on a funnel with ether (3×500 mL) and dried to give crude product (75 g, 94%). No further purification was required for the next reaction.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08093227B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-c8cb6b6bdd17431cbaedc4f6bae64cec |
| 출처 메모 | uspto-grants-2012_01 |