Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 57762806, 화합물

HRID 230647

반응식

HRID 230647 반응식
CN([C:4]([O:8][N:9]1N=NC2C=CC=N[C:10]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:25][N:26]1[CH:30]=[CH:29][N:28]=[C:27]1[C:31]([OH:33])=O.Cl.CNOC.C(N(C(C)C)CC)(C)C>CN(C=O)C>[CH3:10][N:9]([O:8][CH3:4])[C:31]([C:27]1[N:26]([CH3:25])[CH:30]=[CH:29][N:28]=1)=[O:33]

참가 물질

6

반응물 4

HCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 81531DiisopropylethylamineHCID 5576781-methyl-1H-imidazole-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

생성물 1

HCID 57762806HCID 57762806, 화합물수율 212.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

HATU (O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate) (1.75 g; 4.60 mmol) was added in on portion to a stirring solution of 1-methyl-1H-imidazole-2-carboxylic acid (509 mg; 4.04 mmol), N,O-dimethylhydroxylamine hydrochloride (391 mg; 4.01 mmol), and diisopropylethylamine (2.0 mL; 11.9 mmol) in anhydrous DMF (14 mL). The mixture was stirred at room temperature for 17 hours and partitioned between ethyl acetate (100 mL) and water (100 mL). The organic phase was dried (MgSO4) and concentrated in vacuo, giving a colourless oil (1.45 g). This was purified by column chromatography, giving the title compound as a colourless oil (494 mg; 73%).

후처리

  1. custompartitioned between ethyl acetate (100 mL) and water (100 mL)
  2. dry with materialThe organic phase was dried (MgSO4)
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-1b057176fc3b4694a4209927e8cc5045
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566735B2

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