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Diisopropylethylamine → 5,8-Dimethyl-[1,2,4]triazolo[1,5-a]pyrazin-2-ylamine

HRID 1054980
ノート
印刷プレビュー

反応式

HRID 1054980 の反応式
Cl.NO.C([N:7](CC)C(C)C)(C)C.C(OC(=O)[NH:17][C:18](=S)[NH:19][C:20]1[C:25]([CH3:26])=[N:24][CH:23]=[C:22]([CH3:27])[N:21]=1)C>C(O)C.O>[CH3:27][C:22]1[N:21]2[N:7]=[C:18]([NH2:17])[N:19]=[C:20]2[C:25]([CH3:26])=[N:24][CH:23]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 81531DiisopropylethylamineHCID 443297Hydroxyamine hydrochlorideHCID 90017035ethyl-N-[(3,6-dimethylpyrazin-2-yl)carbamothioyl]carbamate

生成物 1

HCID 900260875,8-Dimethyl-[1,2,4]triazolo[1,5-a]pyrazin-2-ylamine収率 71.87%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962
Water
溶媒

反応条件

温度
25 °C

実験手順

A mixture of hydroxylamine hydrochloride (13.68 g, 196.85 mmol) and N,N-diisopropylethylamine (20.6 ml, 118.11 mmol) in ethanol (200 ml) was stirred for 10 minutes at 25° C. To this mixture was then added ethyl-N-[(3,6-dimethylpyrazin-2-yl)carbamothioyl]carbamate (10 g, 39.37 mmol), and the resultant mixture was heated under reflux for 16 hours. The resultant mixture was diluted with water (100 ml), stirred for 10 min, and extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous sodium sulfate, filtered and evaporated. The crude material thus obtained was triturated with hexane affording 5,8-dimethyl-[1,2,4]triazolo[1,5-a]pyrazin-2-ylamine (2.4 g, 71.87%) as a white solid. MS: m/z=164 (M+H+)

後処理

  1. temperatureunder reflux for 16 hours
  2. stirringstirred for 10 min
  3. extractionextracted twice with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customThe crude material thus obtained
  9. customwas triturated with hexane

出典と根拠

ORDレコード
ord-8de2091aaabf40168ebedbcd007daf41
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394311B2

反応ノート

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