참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 4-Amino-3,5-dichlorobenzoic acid | HCID 42061 | — |
| 생성물 | Methyl 4-amino-3,5-dichlorobenzoate | HCID 604808 | 70% |
반응 단계
conc. H2SO4 (2.5 mL, 97.04 mmol) was added drop wise to a stirred solution of 4-amino-3,5-dichlorobenzoic acid (10.0 g, 48.54 mmol) in MeOH (150 mL) at 0° C. and the reaction mixture was then stirred at 80° C. for 8 h. The volatiles were evaporated; ice cold water was added to the residue and which was then extracted with EtOAc. The combined organic layers were washed with brine, dried (Na2SO4), filtered and concentrated under reduced pressure to afford the title compound as a white solid (7.5 g, 70%): 1H NMR (300 MHz, DMSO-d6) δ 8.05 (s, 2H), 3.96 (s, 3H); ESIMS m/z 282 ([M]+); IR (KBr): 1733, 762, 514 cm−1.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09212164B2 |
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| 출처 데이터셋 | uspto-grants-2015_12 |
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| ORD ID | ord-a05d1961b0ed4661b8df8af3859556c1 |
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| 출처 메모 | uspto-grants-2015_12 |
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