Hydroxyamine hydrochloride → 5-Tert-butyl-2-hydroxyl-3-nitro-benzonitrile

HRID 1181925ノート

反応式

HRID 1181925 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([N+:14]([O-:16])=[O:15])[C:8]([OH:13])=[C:9]([CH:12]=1)[CH:10]=O)([CH3:4])([CH3:3])[CH3:2].Cl.[NH2:18]O.C([O-])=O.[Na+]>C(O)=O.O>[C:1]([C:5]1[CH:6]=[C:7]([N+:14]([O-:16])=[O:15])[C:8]([OH:13])=[C:9]([CH:12]=1)[C:10]#[N:18])([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 2723810Sodium FormateHCID 7172095HCID 7172095、化合物

生成物 1

HCID 589806535-Tert-butyl-2-hydroxyl-3-nitro-benzonitrile収率 87.2%

試薬・触媒・溶媒 2

HCID 284Formic Acid溶媒HCID 962Water溶媒

実験手順

The above aldehyde (1.4 g, 6.3 mmol), hydroxylamine hydrochloride (0.438 g, 6.3 mmol), and sodium formate (0.771 g, 11.3 mmol) in formic acid (20 mL) were heated overnight, at reflux, then cooled to room temperature. The reaction was diluted with water, and the resulting precipitate was filtered. The solid was taken up in ether, dried over Na2SO4, filtered and concentrated in vacuo to yield 5-tert-butyl-2-hydroxyl-3-nitro-benzonitrile (1.21 g, 87%) as a yellow solid.

後処理

  1. temperatureat reflux
  2. filtrationthe resulting precipitate was filtered
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-dc4d71ae3b8c4dc18fed4ba13aafebe8
出典データセット
uspto-grants-2007_10
特許番号
US07285545B2

反応ノート

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