참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 3-Hydroxy-2-naphthoic acid | HCID 7104 | — |
| 반응물 | Imipramine Hydrochloride | HCID 8228 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Imipramine | HCID 3696 | 105.5% |
반응 단계
To a solution containing 7.7 g of 3-hydroxy-2-napthoic acid in 75.0 g of USP water was added as necessary dilute HCl or NaOH solution to adjust the solution to about pH 9.4. To a second solution of 13.6 g of imipramine HCl in 100.0 g of USP water was added as necessary dilute HCl or NaOH solution to adjust the solution to about pH 4.5. The imipramine HCl solution was added to the 3-hydroxy-2-napthoic sodium salt solution over a period of about 2 h. The mixture was stirred and held at around 50° C. for approximately 18 h. The mixture was cooled to below about 25° C. and the solids were collected by filtration. The solid cake was washed with USP water (2×100 g). The solid cake was dried at about 105° C. under vacuum to yield a powder (12.7 g) and characterized by DSC (FIG. 13), FTIR (FIG. 14) and 1H NMR (FIG. 15).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08883863B1 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-28456e8ed5094c7dbca468cfb73f22f7 |
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| 출처 메모 | uspto-grants-2014_11 |
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