Sodium Hydroxide → 4-Isobutyloxy-3-nitrobenzoic acid

HRID 851859ノート

反応式

HRID 851859 の反応式
[CH2:1]([O:5][C:6]1[CH:15]=[CH:14][C:9]([C:10]([O:12]C)=[O:11])=[CH:8][C:7]=1[N+:16]([O-:18])=[O:17])[CH:2]([CH3:4])[CH3:3].[OH-].[Na+]>CO.C1COCC1>[CH2:1]([O:5][C:6]1[CH:15]=[CH:14][C:9]([C:10]([OH:12])=[O:11])=[CH:8][C:7]=1[N+:16]([O-:18])=[O:17])[CH:2]([CH3:4])[CH3:3]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 23023853HCID 23023853、化合物

生成物 1

HCID 230238474-Isobutyloxy-3-nitrobenzoic acid収率 98%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 4-isobutyloxy-3-nitrobenzoate (2.50 g, 9.87 mmol) was dissolved in a mixture of methanol (10 mL) and 25 THF (10 mL). After addition of 2M aqueous sodium hydroxide (7.5 mL, 15.0 mmol), the solution was stirred for 18 hours at room temperature. The solvent was distilled off under reduced pressure, and were added to the residue water (20 mL) and 3M aqueous hydrochloric acid to adjust 30 the solution to pH 1. The precipitated crystalline product was collected by filtration. The crystalline product was washed with water (20 mL×2) and dried at 50° C. for 4 hours under reduced pressure, to give 2.31 g (yield 98%) of the desired compound in the form of a white crystalline product.

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionwere added to the residue water (20 mL) and 3M aqueous hydrochloric acid
  3. filtrationThe precipitated crystalline product was collected by filtration
  4. washThe crystalline product was washed with water (20 mL×2)
  5. customdried at 50° C. for 4 hours under reduced pressure

出典と根拠

ORDレコード
ord-72a186cea1e94986b168aa974f6763a2
出典データセット
uspto-grants-2007_08
特許番号
US07253154B2

反応ノート

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