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Hydroxyamine hydrochloride → 4,6-Bis(1,1-dimethylethyl)-5-hydroxy-2-pyrimidine carboxaldehyde oxime

HRID 1742606
ノート
印刷プレビュー

反応式

HRID 1742606 の反応式
[CH3:1][C:2]([C:5]1[C:10]([OH:11])=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[N:8]=[C:7]([CH:16]=O)[N:6]=1)([CH3:4])[CH3:3].Cl.NO.C([O-])(=O)C.[Na+].CC(C1C(O)=CN=C(C=[N:38][OH:39])N=1)(C)C>C(O)C.O>[CH3:1][C:2]([C:5]1[C:10]([OH:11])=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[N:8]=[C:7]([CH:16]=[N:38][OH:39])[N:6]=1)([CH3:4])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 152948964,6-Di-tert-butyl-5-hydroxypyrimidine-2-carbaldehydeHCID 136378411(1,1-Dimethylethyl)-5-hydroxy-2-pyrimidine carboxaldehyde oxime

生成物 1

HCID 1363784134,6-Bis(1,1-dimethylethyl)-5-hydroxy-2-pyrimidine carboxaldehyde oxime

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 962Water溶媒

実験手順

A solution of 4,6-bis(1,1-dimethylethyl)-5-hydroxy-2-pyrimidine carboxaldehyde (1.5 g, 6.3 mmol) , hydroxylamine hydrochloride (2.2 g, 32.7 mmol), and sodium acetate (2.9 g, 34.9 mmol) in ethanol (20 mL) is heated at reflux for 12 hours. The reaction mixture is poured over water (150 mL) and the precipitate is collected by filtration. Recrystallization from ether/hexane gives the desired 4,6-his (1,1-dimethylethyl) -5-hydroxy-2-pyrimidine carboxaldehyde oxime as a mixture of isomers (0.62 g, 39%); mp 205°-220° C.

後処理

  1. temperatureat reflux for 12 hours
  2. filtrationthe precipitate is collected by filtration
  3. customRecrystallization from ether/hexane
  4. customgives the
  5. additionas a mixture of isomers (0.62 g, 39%)

出典と根拠

ORDレコード
ord-a41abdf948d5410cac6fbc8407ce8360
出典データセット
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05340815

反応ノート

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