Hydroxyamine hydrochloride → HCID 178471847, 화합물

HRID 2189782노트

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HRID 2189782 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].Cl.[NH2:20][OH:21].C(=O)(O)[O-].[Na+]>C(O)C>[OH:21][NH:20][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, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

Ethyl 3-(5-cyano-1H-indazol-1-yl)propanoate D47 (3.6 g, 14.80 mmol) was dissolved in ethanol (40 ml), hydroxylamine hydrochloride (2.057 g, 29.6 mmol) and sodium bicarbonate (6.22 g, 74.0 mmol) were added. The mixture was heated at 60° C. overnight. Cooled, filtered and the filtrate was evaporated, dissolved in EtOAc, washed with water (3×20 ml), dried over MgSO4 and evaporated again to give (1.75 g) of product. A further 0.290 g of white crystals were recovered from the rotary evaporater. MS (ES+): C13H16N4O3 requires 276; found (MH+) 277.

후처리

  1. temperatureCooled
  2. filtrationfiltered
  3. customthe filtrate was evaporated
  4. dissolutiondissolved in EtOAc
  5. washwashed with water (3×20 ml)
  6. dry with materialdried over MgSO4
  7. customevaporated again

출처 및 근거

ORD 기록
ord-fc2641e7012e44fab4db1cdf1733347d
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08324254B2

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