참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Methane, dichloromethoxy- | HCID 21004 | — |
| 반응물 | 4-[1-Methyl-1-(1,3-dithiolan-2-yl)ethyl]anisole | HCID 19066444 | — |
| 촉매 | Titanium Tetrachloride | HCID 24193 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Chlorine | HCID 24526 | — |
| 생성물 | 2-Methoxy-5-[1-(1,3-dithiolan-2-yl)-1-methylethyl]benzaldehyde | HCID 19066490 | 30.5% |
반응 단계
To a stirred solution of Compound 80 (0.254 g, 1 mmol) in dry CH2 Cl2 (5 ml) was added a solution of TiCl4 in CH2Cl2 (1M, 3 ml) with cooling (-60° C.). After 3 min., to this was added dichloromethyl methyl ether (0.46 g, 4 mmol) dropwise. The reaction mixture was stirred at same temperature for 1 hr. The mixture was poured into water and stirred at room temperature for 15 min. The organic layer was separated and the aqueous layer was extracted with Et2O (50 ml×2). The combined solution was washed with brine, dried (MgSO4) and concentrated in vacuo to give crude product. The crude product was purified by a column chromatography to give Compound 81 (86 mg) as an oil
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05789423 |
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| 출처 데이터셋 | uspto-grants-1998_08 |
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| ORD ID | ord-eae49ffcc197424ab29aa825a399a947 |
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| 출처 메모 | uspto-grants-1998_08 |
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