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Hydrochloric Acid → HCID 11651470、化合物

HRID 2217796
ノート
印刷プレビュー

反応式

HRID 2217796 の反応式
[CH:1](=O)/[CH:2]=[CH:3]/[CH3:4].[NH2:6][C:7]1[CH:8]=[CH:9][C:10]([Cl:16])=[C:11]([CH:15]=1)[C:12]([OH:14])=[O:13].[N+](C1C=C(S([O-])(=O)=O)C=CC=1)([O-])=O.[Na+].Cl>>[Cl:16][C:10]1[CH:9]=[CH:8][C:7]2[N:6]=[C:3]([CH3:4])[CH:2]=[CH:1][C:15]=2[C:11]=1[C:12]([OH:14])=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 31389Sodium 3-nitrobenzenesulfonateHCID 378795-Amino-2-chlorobenzoic acidHCID 447466Crotonaldehyde

生成物 1

HCID 11651470HCID 11651470、化合物

実験手順

Crotonaldehyde (1.5 mL) was added dropwise over a period of 1 hour to a mixture of 5-amino-2-chlorobenzoic acid (1.7 g), ferrous sulphate heptahydrate (0.77 g), sodium m-nitrobenzenesulphonate (1.2 g) and concentrated hydrochloric acid (11 mL) at 95° C. The reaction mixture was heated for a further 15 minutes then filtered whilst still hot. The collected solid was extracted with boiling 2M aqueous hydrochloric acid solution (20 mL) and the extract combined with the filtrate. Ammonium acetate was then added to give a solution of pH 4, which was cooled in ice and the resultant precipitate collected by filtration and washed with water. The product was converted to its hydrochloride salt by treatment with hydrochloric acid (4M in 1,4-dioxane) and the solid dried in vacuo to give the sub-title compound (0.5 g) as a solid.

後処理

  1. temperatureThe reaction mixture was heated for a further 15 minutes
  2. filtrationthen filtered whilst still hot
  3. extractionThe collected solid was extracted
  4. additionAmmonium acetate was then added
  5. customto give a solution of pH 4, which
  6. temperaturewas cooled in ice
  7. filtrationthe resultant precipitate collected by filtration
  8. washwashed with water
  9. customthe solid dried in vacuo

出典と根拠

ORDレコード
ord-53ab5449d8d24b06ae0251e3d87ed4d1
出典データセット
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07408065B2

反応ノート

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