Potassium Carbonate → 4-chloro-N'-hydroxybenzenecarboximidamide

HRID 59258

반응식

HRID 59258 반응식
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.Cl.[OH:11][NH2:12].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([C:6](=[N:12][OH:11])[NH2:7])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 121634-ChlorobenzonitrileHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 2246504-chloro-N'-hydroxybenzenecarboximidamide수율 40.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 4-chloro benzonitrile (1.000 g, 7.26 mmol) in ethanol (20 mL) was added hydroxyl amine HCl (0.752 g, 10.90 mmol) and potassium carbonate (3.00 g, 21.80 mmol). The reaction mass was refluxed for 10-12 h. Excess of solvent was removed under vacuum and the residue was diluted with water, acidified with dilute HCl. Precipitate obtained was filtered off and sucked dried to afford 0.500 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 5.88 (br s, 2H), 7.42 (d, J=8.1 Hz, 2H), 7.68 (d, J=8.4 Hz, 2H), 9.70 (br s, 1H); MS (m/z): 171.13 (M+H)+.

후처리

  1. temperatureThe reaction mass was refluxed for 10-12 h
  2. customExcess of solvent was removed under vacuum
  3. additionthe residue was diluted with water
  4. customPrecipitate obtained
  5. filtrationwas filtered off
  6. customsucked dried

출처 및 근거

ORD 기록
ord-32820b4765274f828d1aa5ef135e2b1d
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09439890B2

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