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4-Nitrobenzoyl chloride → HCID 18354599、化合物

HRID 1292137
ノート
印刷プレビュー

反応式

HRID 1292137 の反応式
[NH2:1][C:2]1[C:11]([OH:12])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[N+:13]([C:16]1[CH:24]=[CH:23][C:19]([C:20](Cl)=[O:21])=[CH:18][CH:17]=1)([O-:15])=[O:14]>C1(C)C=CC=C(C)C=1>[OH:12][C:11]1[C:2]([NH:1][C:20](=[O:21])[C:19]2[CH:18]=[CH:17][C:16]([N+:13]([O-:15])=[O:14])=[CH:24][CH:23]=2)=[C:3]([CH:8]=[CH:9][CH:10]=1)[C:4]([O:6][CH3:7])=[O:5]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 85024-Nitrobenzoyl chlorideHCID 205248Anthranilic acid, 3-hydroxy-, methyl ester

生成物 1

HCID 18354599HCID 18354599、化合物

試薬・触媒・溶媒 1

HCID 7929M-Xylene溶媒

反応条件

温度
60 °C

実験手順

Methyl 2-amino-3-hydroxybenzoate (0.5 g; 2.99 mmol) was dissolved in m-xylene (40 ml) with warming to 60° C. 4-Nitrobenzoyl chloride (0.556 ml; 2.99 mmol) was added dropwise, and this was left to stir for 4 hours. The solution was cooled to ambient temperature and the m-xylene removed under reduced pressure. The solid was dissolved in water (100 ml) and the organics extracted into ethyl acetate (3×50 ml). The organic fractions were pooled, dried over magnesium sulphate, filtered and the solvent removed under reduced pressure.

後処理

  1. waitthis was left
  2. temperatureThe solution was cooled to ambient temperature
  3. customthe m-xylene removed under reduced pressure
  4. dissolutionThe solid was dissolved in water (100 ml)
  5. extractionthe organics extracted into ethyl acetate (3×50 ml)
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-6969f2d40bab4d2990ba48a3e407df41
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05756510

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート