Hydroxyamine hydrochloride → tert-Butyl 4-(5-bromo-3-((1-(hydroxyamino)ethylidene)amino)pyrazin-2-yl)piperazine-1-carboxylate

HRID 1045747노트

반응식

HRID 1045747 반응식
[Br:1][C:2]1[N:3]=[C:4]([N:21]=[C:22]([N:24](C)C)[CH3:23])[C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1.Cl.N[OH:29]>CO>[Br:1][C:2]1[N:3]=[C:4]([N:21]=[C:22]([NH:24][OH:29])[CH3:23])[C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 58447046tert-Butyl 4-(5-bromo-3-((1-(dimethylamino)ethylidene)amino)pyrazin-2-yl)piperazine-1-carboxylate

생성물 1

HCID 136056833tert-Butyl 4-(5-bromo-3-((1-(hydroxyamino)ethylidene)amino)pyrazin-2-yl)piperazine-1-carboxylate수율 84%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A 100 mL round bottom flask was charged with tert-butyl 4-(5-bromo-3-((1-(dimethylamino)ethylidene)amino)pyrazin-2-yl)piperazine-1-carboxylate (2.8 g, 6.6 mmol) and methanol (25 mL). To the above solution was added hydroxylamine hydrochloride (0.76 g, 10.9 mmol) in one portion. The mixture was stirred at room temperature for 16 h. Work-up: the solvent was evaporated. The resulting crystalline solid was washed with water and collected by filtration. The solid was washed with ethanol (100 mL) and dried, to afford 2.3 g (84%) of the product as a white solid.

후처리

  1. customthe solvent was evaporated
  2. washThe resulting crystalline solid was washed with water
  3. filtrationcollected by filtration
  4. washThe solid was washed with ethanol (100 mL)
  5. customdried

출처 및 근거

ORD 기록
ord-a311399fae5c4b629916340eac4a1378
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569300B2

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