Hydroxyamine hydrochloride → HCID 178471847, 화합물

HRID 2189780노트

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HRID 2189780 반응식
[C:1]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[N:7]=[CH:6]2)#[N:2].C(=O)(O)[O-].[Na+].Cl.[NH2:25][OH:26]>C(O)C>[OH:26][NH:25][C:1](=[NH:2])[C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[N:7]=[CH:6]2

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 59316705Ethyl 3-(5-cyano-1H-indazol-1-yl)propanoate

생성물 1

HCID 178471847HCID 178471847, 화합물수율 67.3%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
50 °C

실험 절차

Ethyl 3-(5-cyano-1H-indazol-1-yl)propanoate (D47) (1 g, 4.11 mmol) was dissolved in ethanol (30 ml) and sodium bicarbonate (1.73 g, 20.88 mmol) and hydroxylamine hydrochloride (571 mg, 8.22 mmol) were added. The reaction was left at room temperature overnight and then heated to 50° C. for 4 hours then left to cool overnight. The reaction mixture was filtered and the residue washed with ethanol. The ethanolic filtrate was evaporated to dryness in vacuo and then triturated with ether to give the title compound (764 mg) as a white solid of approximately 90% purity. MS (ES): C13H16N4O3 requires 276; found (MH+) 277.

후처리

  1. waitthen left
  2. temperatureto cool overnight
  3. filtrationThe reaction mixture was filtered
  4. washthe residue washed with ethanol
  5. customThe ethanolic filtrate was evaporated to dryness in vacuo
  6. customtriturated with ether

출처 및 근거

ORD 기록
ord-a5111fba89db4246940d52fb00a03d7a
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08324254B2

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