Sodium Methoxide → N-[2-(5-amino-1-methylpyrazol-4-yl)ethyl]formamide

HRID 349530노트

반응식

HRID 349530 반응식
Cl.Cl.[NH2:3][C:4]1[N:8]([CH3:9])[N:7]=[CH:6][C:5]=1[CH2:10][CH2:11][NH2:12].[CH3:13][O-:14].[Na+]>CO>[NH2:3][C:4]1[N:8]([CH3:9])[N:7]=[CH:6][C:5]=1[CH2:10][CH2:11][NH:12][CH:13]=[O:14]

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 179619764-(2-Aminoethyl)-1-methyl-1H-pyrazol-5-amine dihydrochloride

생성물 1

HCID 17962016N-[2-(5-amino-1-methylpyrazol-4-yl)ethyl]formamide

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of 2-(5-amino-1-methylpyrazol-4-yl)ethylamine dihydrochloride (2.98 g, 14 mmol) in methanol (50 ml) was added 28% sodium methoxide solution in methanol (5.4 ml, 28 mmol). The mixture was filtered through Celite, and the filtrate was concentrated in vacuo. A mixture of the residue and ethyl formate (80 ml) was stirred under reflux for 16 hours. To the reaction mixture was added chloroform, and the mixture was filtered through Celite. The filtrate was concentrated in vacuo to give N-[2-(5-amino-1-methylpyrazol-4-yl)ethyl]formamide (2.7 g) as a brown oil. 1H-NMR(CDCl3) δ2.57 (2H, t, J=6.9 Hz), 3.40–3.44 (2H, m), 3.67(3H, s), 5.77 (1H, br), 7.15 (1H, s), 8.16 (1H, s)

후처리

  1. filtrationThe mixture was filtered through Celite
  2. concentrationthe filtrate was concentrated in vacuo
  3. additionA mixture of the residue and ethyl formate (80 ml)
  4. temperatureunder reflux for 16 hours
  5. additionTo the reaction mixture was added chloroform
  6. filtrationthe mixture was filtered through Celite
  7. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-f28bde5c0d784326a4183e55f98b970d
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179801B2

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