참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Trimethylphosphine | HCID 68983 | — |
| 반응물 | 7-(1-azidoethyl)-3-methyl-6-phenyl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one | HCID 86650064 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 7-(1-aminoethyl)-3-methyl-6-phenyl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one | HCID 66863135 | — |
반응 단계
To a stirred solution of 7-(1-azidoethyl)-3-methyl-6-phenyl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one (0.044 g, 0.14 mmol) in tetrahydrofuran (0.4 mL) and water (0.102 mL) was added 1.0 M of trimethylphosphine in tetrahydrofuran (0.17 mL) at room temperature and the mixture was stirred at room temperature for 1 hour. To the mixture was added EtOAc and the mixture was extracted twice with 1 N HCl. The combined extracts were neutralized with solid sodium bicarbonate and extracted with methylene chloride. The combined organic layers were washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was used directly in next step (36 mg, 89.3%). LCMS calculated for C15H16N3OS (M+H)+: m/z=286.1. Found: 286.0.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09434746B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-68fe3d97b3d246b8936a1e5f06c6621c |
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| 출처 메모 | uspto-grants-2016_09 |
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