Water → 5-[(Hydroxyimino)methyl]-3-thiophenecarbonitrile

HRID 1582900노트

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HRID 1582900 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=O)[S:6][CH:7]=1)#[N:2].C(=O)([O-])[O-].[Na+].[Na+].Cl.[NH2:17][OH:18].O>CO>[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=[N:17][OH:18])[S:6][CH:7]=1)#[N:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 122800095-Formylthiophene-3-carbonitrile

생성물 1

HCID 738516325-[(Hydroxyimino)methyl]-3-thiophenecarbonitrile수율 97.1%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
10 °C

실험 절차

11.6 g (84.6 mmol) of 4-cyanothiophene-2-carbaldehyde were dissolved in 140 ml of methanol and 12.3 g (116.1 mmol) of sodium carbonate were added. 6.5 [lacuna] (93.5 mmol) of hydroxylamine hydrochloride were subsequently added at 15° C. with cooling, a little at a time, and the mixture was stirred for 2 hours at 10° C. After 80 ml of water had been added, the reaction mixture was extracted five times using in each case 50 ml of diethyl ether, the organic phase was dried over sodium sulfate and the solvent was removed in vacuo. 12.5 g of the required product resulted as a yellow crystal powder (96% of theory).

후처리

  1. temperaturewith cooling
  2. extractionthe reaction mixture was extracted five times
  3. dry with materialthe organic phase was dried over sodium sulfate
  4. customthe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-428f6cf68ce44ccd90b0424d6b713a43
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06740647B1

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