참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 반응물 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 반응물 | 2-Bromo-4-(bromomethyl)benzaldehyde | HCID 12016038 | — |
| 반응물 | Di-tert-butyl phosphite | HCID 21959072 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Di(tert-butyl) [2-bromo-4-(bromomethyl)phenyl](hydroxy)methylphosphonate | HCID 12016039 | 89% |
반응 단계
Di-tert-butyl phosphite (14.8 g, 76.3 mmol, 1.05 eq) was dissolved in 200 ml THF at −78° C. under nitrogen and 72 ml (1.05 eq) of 1.06M Lithium bis(trimethylsilyl)amide in THF was added over 30 min. The mixture was left stirring at −78° C. under nitrogen for 30 min and then added to a solution of the compound of Step 3 (20.2 g, 72.7 mmol, 1 eq) in 200 ml THF at −78° C. The solution was warmed to 0° C. and then poured into 400 ml of half saturated aqueous ammonium acetate. The layers were separated and the aqueous layer was washed with 400 ml isopropyl acetate. The organic layers were combined, dried with sodium sulfate and the solvent removed. The crude solid was then triturated with 15% EtOAc/hexane for 2 hours and 30.4 g (89%) of the title compound was obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06777433B2 |
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| 출처 데이터셋 | uspto-grants-2004_08 |
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| ORD ID | ord-9d72a0551e864d5489519bd0482b2197 |
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| 출처 메모 | uspto-grants-2004_08 |
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