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Hydrochloric Acid → Methyl 2-amino-3-nitro-4-(trifluoromethyl)benzoate

HRID 1698601
ノート
印刷プレビュー

反応式

HRID 1698601 の反応式
C([NH:4][C:5]1[C:14]([N+:15]([O-:17])=[O:16])=[C:13]([C:18]([F:21])([F:20])[F:19])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=O)C.Cl>CO>[NH2:4][C:5]1[C:14]([N+:15]([O-:17])=[O:16])=[C:13]([C:18]([F:19])([F:20])[F:21])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8]
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 313Hydrochloric AcidHCID 67272857Methyl 2-(acetylamino)-3-nitro-4-(trifluoromethyl)benzoate

生成物 1

HCID 67272484Methyl 2-amino-3-nitro-4-(trifluoromethyl)benzoate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
55 °C

実験手順

A mixture of methyl 2-(acetylamino)-3-nitro-4-(trifluoromethyl)benzoate (1.00 g, 3.27 mmol) and 10% hydrochloric acid in methanol solution (10 ml) was heated at 55° C. for 16 h. The reaction mixture was concentrated in vacuo. The residue was diluted with aqueous saturated sodium bicarbonate and extracted with ethyl acetate. The extracts were washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel with a 30% ethyl acetate/n-hexane to give 780 mg (0.030 mol 90%) of the title compound as a yellow powder.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionThe residue was diluted with aqueous saturated sodium bicarbonate
  3. extractionextracted with ethyl acetate
  4. washThe extracts were washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography on silica gel with a 30% ethyl acetate/n-hexane

出典と根拠

ORDレコード
ord-e52db10c80dd437798113264bed85c83
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163935B2

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