참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Bromo-4-iodobenzene | HCID 11522 | — |
| 반응물 | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| 반응물 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 8-(4-Bromophenyl)-1,4-dioxa-8-azaspiro[4.5]decane | HCID 12169341 | 58.8% |
반응 단계
0.5 g of 1-bromo-4-iodobenzene and 0.3 g of 1,4-dioxa-8-azaspiro[4.5]decane are placed in 10 ml of toluene and then 0.08 g of tris(dibenzylideneacetone)dipalladium(0), 0.061 g of 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene and 0.255 g of sodium tert-butoxide are added. The reaction medium is brought to reflux of the solvent for 4 h. Ethyl acetate is subsequently added and the mixture is washed twice with water and once with a saturated aqueous sodium chloride solution. The organic phase is dried over magnesium sulphate and concentrated under reduced pressure. The crude product obtained is chromatographed on silica gel, elution being carried out with a heptane/ethyl acetate (4/1) solvent mixture. 0.31 g of 8-(4-bromophenyl)-1,4-dioxa-8-azaspiro[4.5]decane is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08530657B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_09 |
|---|
| ORD ID | ord-bfdb6ef5a9a9453989e933069f5009fe |
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| 출처 메모 | uspto-grants-2013_09 |
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