Hydroxyamine hydrochloride → HCID 178436634、化合物

HRID 1924829ノート

反応式

HRID 1924829 の反応式
CC([O-])(C)C.[K+].Cl.[NH2:8][OH:9].[CH2:10]([C:12]1[CH:13]=[C:14]([CH:17]=[C:18]([CH3:20])[N:19]=1)[C:15]#[N:16])[CH3:11]>CO>[CH2:10]([C:12]1[CH:13]=[C:14]([CH:17]=[C:18]([CH3:20])[N:19]=1)[C:15]([NH:8][OH:9])=[NH:16])[CH3:11]

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 23665647Potassium tert-butoxideHCID 670270042-Ethyl-6-methylisonicotinonitrile

生成物 1

HCID 178436634HCID 178436634、化合物収率 108.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

At 0° C., KOtBu (1.81 g, 16.2 mmol) is carefully added to methanol (25 mL). Hydroxylamine hydrochloride (963 mg, 13.9 mmol) is then added to this solution. The suspension is stirred for 30 min before 2-ethyl-6-methyl-isonicotinonitrile (675 mg, 4.62 mmol) is added. The mixture is refluxed for 1 h, the solvent is evaporated. The residue is dissolved in water, extracted three times with EA. The org. extracts are dried over MgSO4, filtered, evaporated and dried under HV to give 2-ethyl-N-hydroxy-6-methyl-isonicotinamidine (897 mg) as a white powder, LC-MS: tR=0.31 min, [M+1]+=180.32.

後処理

  1. additionis added
  2. temperatureThe mixture is refluxed for 1 h
  3. customthe solvent is evaporated
  4. dissolutionThe residue is dissolved in water
  5. extractionextracted three times with EA
  6. dry with materialextracts are dried over MgSO4
  7. filtrationfiltered
  8. customevaporated
  9. customdried under HV

出典と根拠

ORDレコード
ord-247efcd1836245d7910b02d86dcdb6ee
出典データセット
uspto-grants-2012_05
特許番号
US08178562B2

反応ノート

読み込み中…