Hydroxyamine hydrochloride → HCID 178436634, 화합물

HRID 1924829노트

반응식

HRID 1924829 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 178436634HCID 178436634, 화합물수율 108.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-247efcd1836245d7910b02d86dcdb6ee
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178562B2

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