Potassium Carbonate → 4-chloro-N'-hydroxybenzenecarboximidamide

HRID 59258

反応式

HRID 59258 の反応式
[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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 121634-ChlorobenzonitrileHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 2246504-chloro-N'-hydroxybenzenecarboximidamide収率 40.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-32820b4765274f828d1aa5ef135e2b1d
出典データセット
uspto-grants-2016_09
特許番号
US09439890B2

関連ノート

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