Hydroxyamine hydrochloride → HCID 178471847、化合物

HRID 2189781ノート

反応式

HRID 2189781 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178471847HCID 178471847、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

Ethyl 3-(5-cyano-1H-indazol-1-yl)propanoate (D47) (3.84 g, 15.8 mmol) was dissolved in ethanol (100 ml) and sodium bicarbonate (6.6 g, 79 mmol) and then hydroxylamine hydrochloride (3.3 g, 47.4 mmol) were added. The reaction was heated to 50° C. for a total of 11 hours and then left to cool overnight. The reaction was filtered and the residue washed with ethanol. The filtrate was evaporated to dryness in vacuo and the resultant solid triturated with ether to generate the title compound (3.79 g) as a white solid. MS (ES): C13H16N4O3 requires 276; found (MH+) 277.

後処理

  1. waitleft
  2. temperatureto cool overnight
  3. filtrationThe reaction was filtered
  4. washthe residue washed with ethanol
  5. customThe filtrate was evaporated to dryness in vacuo
  6. customthe resultant solid triturated with ether

出典と根拠

ORDレコード
ord-799d95a2309f4ed4acc65eada05d0b08
出典データセット
uspto-grants-2012_12
特許番号
US08324254B2

反応ノート

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