Isovaleric Acid → HCID 21504713, 화합물

HRID 2202877노트

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HRID 2202877 반응식
[Br:1][C:2]1[CH:7]=[C:6]([NH:8][CH3:9])[C:5]([NH2:10])=[CH:4][CH:3]=1.[C:11](O)(=O)[CH2:12][CH:13]([CH3:15])[CH3:14].C(N(CC)C(C)C)(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[Cl-].[Cl-].[Ca+2]>CN(C=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:10]=[C:11]([CH2:12][CH:13]([CH3:15])[CH3:14])[N:8]([CH3:9])[C:6]=2[CH:7]=1

참가 물질

7

반응물 5

HCID 10430Isovaleric AcidHCID 81531DiisopropylethylamineHCID 5284359Calcium ChlorideHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 121982705-Bromo-N1-methylbenzene-1,2-diamine

생성물 1

HCID 21504713HCID 21504713, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

To a solution of 5-bromo-N1-methylbenzene-1,2-diamine (159 mg), isovaleric acid (0.087 ml) and N,N-diisopropylethylamine (0.41 ml) in DMF (2 ml) was added HATU (316 mg) at room temperature. The mixture was stirred at room temperature under a dry atmosphere (CaCl2 tube) for 3 h. After evaporation of the mixture, the residue was purified by NH silica gel column chromatography (hexane/EtOAc). The resulting residue was stirred in AcOH (2.0 ml) at 80° C. for 1 h. After evaporation, the residue was purified by NH silica gel column chromatography (hexane/EtOAc) to give the title compound (156 mg) as a pale yellow solid.

후처리

  1. customAfter evaporation of the mixture
  2. customthe residue was purified by NH silica gel column chromatography (hexane/EtOAc)
  3. customAfter evaporation
  4. customthe residue was purified by NH silica gel column chromatography (hexane/EtOAc)

출처 및 근거

ORD 기록
ord-eabc449f317f4e259a4b46258dc29b2c
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09365540B2

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