Hydroxyamine hydrochloride → (S)-tert-Butyl 4-(5-Aminopyrazin-2-yl)-3-methylpiperazine-1-carboxylate

HRID 1022000노트

반응식

HRID 1022000 반응식
C1(C(=[N:14][C:15]2[N:16]=[CH:17][C:18]([N:21]3[CH2:26][CH2:25][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:23][C@@H:22]3[CH3:34])=[N:19][CH:20]=2)C2C=CC=CC=2)C=CC=CC=1.C([O-])(=O)C.[Na+].Cl.NO>CO>[NH2:14][C:15]1[N:16]=[CH:17][C:18]([N:21]2[CH2:26][CH2:25][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:23][C@@H:22]2[CH3:34])=[N:19][CH:20]=1

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 86684427(S)-tert-Butyl 4-(5-(Diphenylmethyleneamino)pyrazin-2-yl)-3-methylpiperazine-1-carboxylate

생성물 1

HCID 86684428(S)-tert-Butyl 4-(5-Aminopyrazin-2-yl)-3-methylpiperazine-1-carboxylate수율 64%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 230b (3.3 g, 7.2 mmol) in methanol (25 mL) were added sodium acetate (708 mg, 8.6 mmol) and hydroxylamine hydrochloride (907 mg, 8.6 mmol). The reaction mixture was stirred for 0.5 h. It was then concentrated in vacuo. The residue was purified by silica-gel column chromatography eluting with dichloromethane/methanol (50:1 to 30:1) to afford 230c as yellow oil (1.35 g, 64%). MS: [M+H]+ 294.3.

후처리

  1. concentrationIt was then concentrated in vacuo
  2. customThe residue was purified by silica-gel column chromatography
  3. washeluting with dichloromethane/methanol (50:1 to 30:1)

출처 및 근거

ORD 기록
ord-a600b44577a04df7a9012b0ab4f7c4ca
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716274B2

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