Hydroxyamine hydrochloride → HCID 58446972, 화합물

HRID 1045773노트

반응식

HRID 1045773 반응식
[Br:1][C:2]1[C:3]([N:21]=[CH:22][N:23](C)C)=[N:4][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:28]>CO>[Br:1][C:2]1[C:3]([N:21]=[CH:22][NH:23][OH:28])=[N:4][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 58447035HCID 58447035, 화합물

생성물 1

HCID 58446972HCID 58446972, 화합물수율 80%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A 100 mL round bottom flask was charged with tert-butyl 4-(5-bromo-4-(((dimethylamino)methylene)amino)pyrimidin-2-yl)piperazine-1-carboxylate (2.0 g) and methanol (30 mL). To the above solution was added hydroxylamine hydrochloride (0.5 g, 7.3 mmol) in one portion. The resulting mixture was stirred at room temperature for 12 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 1.0 g (80%) 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-f21145a0dee544949b45b2a072cc5e23
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569300B2

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