Hydroxylamine → HCID 178526331, 화합물

HRID 574697

반응식

HRID 574697 반응식
[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

참가 물질

6

반응물 4

HCID 787HydroxylamineHCID 8857Ethyl AcetateHCID 23665404Sodium Acetate TrihydrateHCID 178418743HCID 178418743, 화합물

생성물 1

HCID 178526331HCID 178526331, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bde9e35a5f2449c097bc85ff4f41d369
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034907B2

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