참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Morpholine, 4-(2-chloro-4-nitrophenyl)- | HCID 108711 | — |
| 촉매 | Iron | HCID 23925 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 3-Chloro-4-morpholinoaniline | HCID 108661 | 71.4% |
반응 단계
To a mixture of concentrated hydrochloric acid (1.0 mL) and water (50 mL) was added iron powder (7.55 g, 135 mmol) in one portion and the mixture was stirred at 65° C. for 15 min. The aqueous layer of the mixture was poured out and a solution of 4-(2-chloro-4-nitrophenyl)morpholine (3.28 g, 13.5 mmol) in MeOH (50 mL) was added to the above processed iron powder. The mixture was acidified to pH 3 with hydrochloric acid and stirred further at 65° C. for 45 min. The mixture was then cooled to rt, adjusted to pH 10 with Et3N and filtered and the filtrate was concentrated in vacuo. The residue was dissolved in DCM (150 mL) and the solution was washed with water (100 mL×3) and brine (100 mL), dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound as a white solid (2.05 g, 71%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09434695B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-06b1569164fa437880b489155b479a9c |
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| 출처 메모 | uspto-grants-2016_09 |
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