참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tin tetrachloride | HCID 24287 | — |
| 반응물 | beta-D-Ribofuranoside, methyl 2,3,5-tris-O-[(2,4-dichlorophenyl)methyl]- | HCID 11767425 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-o-Methyl-3,5-bis-o-(2,4-dichlorobenzyl)-beta-d-ribofuranose | HCID 67435068 | — |
반응 단계
To a solution of the product of Step 1 (171.60 g, 0.2676 mol) in 1.8 L CH2Cl2 that was cooled to 0° C., was added dropwise a solution of stannous chloride (31.522 mL, 0.2676 mol) in 134 mL CH2Cl2 while stirring. After the solution was kept at 3° C. for 27 hours, another 5.031 ml of SnCl4 (0.04282 mol) was added and the solution was kept at 3° C. overnight. After 43 hours the reaction was quenched by carefully adding the solution to 1.9 L saturated NaHCO3 solution. Tin salts were removed via filtration through celite after which the organic phace was isolated, dried with MgSO4 and evaporated in vacuo. The yield of raw, dark yellow oil was 173.6 g, which contains 2,4-dibenzoyl chloride. The crude oil was used directly in the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07094768B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-72933cad450b4014b6b24b165b8c5239 |
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| 출처 메모 | uspto-grants-2006_08 |
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