Water → Methyl 2-chloro-3-nitrobenzoate

HRID 51342

反応式

HRID 51342 の反応式
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].IC.[C:16](=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH3:16])=[O:5]

参加物

6

実験手順

A solution of 2-chloro-3-nitrobenzoic acid (20.16 g, 100.0 mM), iodomethane (15.6 g, 110 mM), and potassium carbonate (15.0 g, 108.5 mM) in 100 mL DMF was stirred at room temperature for 48 hours. The mixture was poured into 1.5 liters of H2O. The resultant precipitate was collected by 20.0 g (93%) of methyl 2-chloro-3-nitrobenzoate as a white solid. 1H NMR (CDCl3) δ8.42 (dd, 1H, J=1 and 8 Hz), 8.18 (dd, 1H, J=1 and 8 Hz), 7.43 (t, 1H, J=8 Hz), and 3.9 (s, 3H). IR (KBr, cm−1) 1743, 1719, 1595, 1540, 1532, 1433, 1357, 1300, and 730. MS (FD) m/e 215, 216.

後処理

  1. customThe resultant precipitate was collected by 20.0 g (93%) of methyl 2-chloro-3-nitrobenzoate as a white solid

出典と根拠

ORDレコード
ord-f780d5d858d743999bf339447a4565cd
出典データセット
uspto-grants-2004_03
特許番号
US06713645B1

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