Hydroxylamine → HCID 178526331、化合物

HRID 574697

反応式

HRID 574697 の反応式
[NH:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH:10]=O)=[CH:9][C:4]=2[N:3]=[CH:2]1.[NH2:12][OH:13].O.O.O.C([O-])(=O)C.[Na+].C(OCC)(=O)C>CO>[NH:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH:10]=[N:12][OH:13])=[CH:9][C:4]=2[N:3]=[CH:2]1

参加物

6

反応物 4

HCID 787HydroxylamineHCID 8857Ethyl AcetateHCID 23665404Sodium Acetate TrihydrateHCID 178418743HCID 178418743、化合物

生成物 1

HCID 178526331HCID 178526331、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1H-benzo[d]imidazole-5-carbaldehyde (0.57 mmol, 1 eq.) was dissolved in 5 mL methanol, hydroxylamine (0.68 mmol, 1.2 eq.) and sodium acetate trihydrate (0.68 mmol, 1.2 eq.) were added. The mixture was stirred for 1 hour at ambient temperature. 20 mL Ethyl acetate was added and the organic layer was washed with 20 mL of brine. The organic layer was dried over magnesium sulfate, filtrated and the solvent was removed under reduced pressure. The product was purified by means of flash-chromatography using silica gel and a ethyl acetate/MeOH-gradient.

後処理

  1. washthe organic layer was washed with 20 mL of brine
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationfiltrated
  4. customthe solvent was removed under reduced pressure
  5. customThe product was purified by means of flash-chromatography

出典と根拠

ORDレコード
ord-bde9e35a5f2449c097bc85ff4f41d369
出典データセット
uspto-grants-2015_05
特許番号
US09034907B2

関連ノート

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