Hydroxyamine hydrochloride → 5-Bromo-2-nitrothiophene-3-carbaldehyde oxime

HRID 385712

反応式

HRID 385712 の反応式
[Br:1][C:2]1[S:6][C:5]([N+:7]([O-:9])=[O:8])=[C:4]([CH:10]=O)[CH:3]=1.Cl.[NH2:13][OH:14].C([O-])(=O)C.[Na+]>C(O)C>[Br:1][C:2]1[S:6][C:5]([N+:7]([O-:9])=[O:8])=[C:4]([CH:10]=[N:13][OH:14])[CH:3]=1

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 534029475-Bromo-2-nitrothiophene-3-carbaldehyde

生成物 1

HCID 723159975-Bromo-2-nitrothiophene-3-carbaldehyde oxime

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5-Bromo-2-nitrothiophene-3-carbaldehyde (22.5 g, 95 mmol), hydroxylamine hydrochloride (6.96 g, 100 mmol) and sodium acetate (8.21 g, 100 mmol) were stirred in ethanol (225 mL) at room temperature overnight. The solvent was removed in vacuo, saturated NaHCO3 was added and the products extracted into EtOAc (3×). The combined organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo to give the title compound as an orange solid.

後処理

  1. customThe solvent was removed in vacuo, saturated NaHCO3
  2. additionwas added
  3. extractionthe products extracted into EtOAc (3×)
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4691dfd4a98b4a58809149e9cf146357
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

関連ノート

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