참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzoic acid, 3-methyl-2-nitro-, methyl ester | HCID 79621 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Methyl 3-methylanthranilate | HCID 2763406 | 97.5% |
반응 단계
Methyl 3-methyl-2-nitrobenzoate (98.5 g, 505 mmol), 5% Pd/C (Degussa CE 105 XRC/W, 1.0 g), and acetonitrile (300 mL) were combined in a 600-mL pressure vessel. The mixture was heated to 70° C. and hydrogenated at 65 psi (450 kPa) for 8 h. More 5% Pd/C (1.0 g) was added and hydrogenation was continued at 100 psi (690 kPa) for 8.5 h. Then the reaction mixture was cooled, purged with nitrogen, and filtered through Celite® diatomaceous filter aid, rinsing with acetonitrile (3×25 mL). The combined filtrates were partly evaporated to a weight of ˜160 g, and then diluted with acetonitrile to a total weight of 200g. Quantitative HPLC of this solution showed 40.3 wt % of the title compound (80.6 g, 97.5% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07528260B2 |
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| 출처 데이터셋 | uspto-grants-2009_05 |
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| ORD ID | ord-ab13717415004796982f64776a49a673 |
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| 출처 메모 | uspto-grants-2009_05 |
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