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

HRID 1181925노트

반응식

HRID 1181925 반응식
[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]

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 2723810Sodium FormateHCID 7172095HCID 7172095, 화합물

생성물 1

HCID 589806535-Tert-butyl-2-hydroxyl-3-nitro-benzonitrile수율 87.2%

시약·촉매·용매 2

HCID 284Formic Acid용매HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-dc4d71ae3b8c4dc18fed4ba13aafebe8
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285545B2

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