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2-(1-Methylethoxy)-5-nitrobenzoic acid → 5-Amino-2-isopropoxybenzoic acid

HRID 1096589
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HRID 1096589 반응식
[CH:1]([O:4][C:5]1[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][C:6]=1[C:7]([OH:9])=[O:8])([CH3:3])[CH3:2]>CCO.[Pd]>[NH2:14][C:11]1[CH:12]=[CH:13][C:5]([O:4][CH:1]([CH3:3])[CH3:2])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8]
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참가 물질

4

반응물 1

HCID 44473202-(1-Methylethoxy)-5-nitrobenzoic acid

생성물 1

HCID 160422975-Amino-2-isopropoxybenzoic acid수율 79.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

Methyl 2-isopropoxy-5-nitrobenzoate (6.92 g, 28.95 mmol) was taken up in THF/H2O (35 ml of each) and LiOH (1.39 g, 57.9 mmol) was added. The mixture was stirred at RT overnight then the pH was lowered to 1 by the addition of concentrated HCl and the product extracted in ethyl acetate (50 ml). The organic layer was dried (MgSO4) and evaporated to give 2-isopropoxy-5-nitrobenzoic acid (6.02 g, 92.5%) as a yellow solid. 1H NMR (δ, 250 MHz, DMSO-d6): 1.32 (d, 6-H, CH3), 4.88 (septet, 1-H, CH), 7.37 (d, 1-H, aromatic), 8.32 (dd, 1-H, aromatic), 8.40 (d, 1-H, aromatic), 13.13 (s, 1-H, CO2H). 2-Isopropoxy-5-nitrobenzoic acid (6.02 g, 26.75 mmol) was suspended in EtOH (100 ml) and 10% Pd on C (wet basis) (600 mg) was added. The mixture was hydrogenated at 50 psi for 2 hrs. The mixture was filtered through celite and the volatiles were removed in vacuo. The residue was triturated with IPA, and the resulting solid filtered off, washed with MTBE and dried in vacuo to give 4.15 g of 5-amino-2-isopropoxybenzoic acid (79.5%) as a pale yellow solid.

후처리

  1. filtrationThe mixture was filtered through celite
  2. customthe volatiles were removed in vacuo
  3. customThe residue was triturated with IPA
  4. filtrationthe resulting solid filtered off
  5. washwashed with MTBE
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-cf488f5824bf4ba38375c870d8a283bf
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08138357B2

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