Hydrogen Peroxide → 3-(3-Chloropropoxy)-4-methoxy-6-nitrobenzoic acid

HRID 1803020ノート

反応式

HRID 1803020 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([C:11]([N+:16]([O-:18])=[O:17])=[CH:12][C:13]=1[O:14][CH3:15])[CH:9]=[O:10].[OH-:19].[Na+].OO>CO>[Cl:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([C:11]([N+:16]([O-:18])=[O:17])=[CH:12][C:13]=1[O:14][CH3:15])[C:9]([OH:19])=[O:10]

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 14798Sodium Hydroxide2 回HCID 250518443-(3-Chloropropoxy)-4-methoxy-6-nitrobenzaldehyde

生成物 1

HCID 230330043-(3-Chloropropoxy)-4-methoxy-6-nitrobenzoic acid収率 86%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methanol (4 lt), 3-(3-chloropropoxy)-4-methoxy-6-nitro benzaldehyde (560 gm) and 30% methanolic NaOH solution (5 ml) were heated to 45° C. To this reaction mass 35% of H2O2 solution (1200 ml) was added drop wise in 3-4 hours maintaining a pH of 10.5-11.5 with 30% methanolic NaOH solution. The reaction mass was quenched into ice water (10 kg) and the pH adjusted to 2.0-3.0 using hydrochloric acid. The solid obtained was filtered, washed with 50% aqueous methanol (500 ml) and dried at 45-50° C. to yield the title compound (510 gm, 86% yield).

後処理

  1. customThe reaction mass was quenched into ice water (10 kg)
  2. customThe solid obtained
  3. filtrationwas filtered
  4. washwashed with 50% aqueous methanol (500 ml)
  5. customdried at 45-50° C.

出典と根拠

ORDレコード
ord-9e41eda3d26c4256933a81a477637ade
出典データセット
uspto-grants-2013_01
特許番号
US08350029B2

反応ノート

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