참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | N-Propylpiperazinium dibromide | HCID 3085288 | — |
| 반응물 | 1-Chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine | HCID 19799606 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | HCID 19799597 | HCID 19799597 | 59.5% |
반응 단계
A mixture of 2.8 g (0.01 mole of 3-[3-(trifluoromethyl) phenoxy]-1-azetidinecarbonyl chloride and 4.2 g (0.03 mole) of potassium carbonate in 25 ml of tetrahydrofuran was stirred for 10 min, then treated with 2.9 g (0.01 mole) of 1-propylpiperazine dihydrobromide in small portions. After 30 min, a few pieces of ice were added. After stirring for 17 hr, the reaction was diluted with 200 ml of water then extracted with methylene chloride (2×50 ml). The combined extracts were dried over magnesium sulfate and concentrated in vacuo, yielding 4.84 g of crude residue. The residue was converted to the fumarate salt in 2-propanol, concentrated to a solid in vacuo and recrystallized from acetone with a trace of ethanol to yield 2.9 g (59.5%) of fine white crystals; m.p 117°-123° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05068231 |
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| 출처 데이터셋 | uspto-grants-1991_11 |
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| ORD ID | ord-1b26e8713e0641c9b4c07d75148a8592 |
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| 출처 메모 | uspto-grants-1991_11 |
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