Hydroxyamine hydrochloride → HCID 58446972、化合物

HRID 1045773ノート

反応式

HRID 1045773 の反応式
[Br:1][C:2]1[C:3]([N:21]=[CH:22][N:23](C)C)=[N:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1.Cl.N[OH:28]>CO>[Br:1][C:2]1[C:3]([N:21]=[CH:22][NH:23][OH:28])=[N:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 58447035HCID 58447035、化合物

生成物 1

HCID 58446972HCID 58446972、化合物収率 80%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 100 mL round bottom flask was charged with tert-butyl 4-(5-bromo-4-(((dimethylamino)methylene)amino)pyrimidin-2-yl)piperazine-1-carboxylate (2.0 g) and methanol (30 mL). To the above solution was added hydroxylamine hydrochloride (0.5 g, 7.3 mmol) in one portion. The resulting mixture was stirred at room temperature for 12 h. Work-up: the solvent was evaporated. The resulting crystalline solid was washed with water and collected by filtration. The solid was washed with ethanol (100 mL) and dried, to afford 1.0 g (80%) of the product as a white solid.

後処理

  1. customthe solvent was evaporated
  2. washThe resulting crystalline solid was washed with water
  3. filtrationcollected by filtration
  4. washThe solid was washed with ethanol (100 mL)
  5. customdried

出典と根拠

ORDレコード
ord-f21145a0dee544949b45b2a072cc5e23
出典データセット
uspto-grants-2013_10
特許番号
US08569300B2

反応ノート

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