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Lithium Hydroxide → HCID 68455974, 화합물

HRID 2357653
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HRID 2357653 반응식
[C:1]([C:3]1[C:12]2[C:7](=[CH:8][C:9]([C:13]3[CH:14]=[C:15]([CH:20]=[CH:21][C:22]=3[CH3:23])[C:16](OC)=[O:17])=[CH:10][CH:11]=2)[CH:6]=[N:5][N:4]=1)#[N:2].[Li+].[OH-:25].CN(C(ON1N=NC2[CH:37]=[CH:38][CH:39]=[N:40]C1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C1(N)CC1>C1COCC1.O.C(OCC)(=O)C>[CH:39]1([NH:40][C:16]([C:15]2[CH:20]=[CH:21][C:22]([CH3:23])=[C:13]([C:9]3[CH:8]=[C:7]4[C:12](=[CH:11][CH:10]=3)[C:3]([C:1]([NH2:2])=[O:25])=[N:4][N:5]=[CH:6]4)[CH:14]=2)=[O:17])[CH2:37][CH2:38]1
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7

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HCID 3939Lithium HydroxideHCID 69828CyclopropylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 68455479HCID 68455479, 화합물

생성물 1

HCID 68455974HCID 68455974, 화합물

시약·촉매·용매 2

HCID 8857
Ethyl Acetate
용매
HCID 21881883Oxolane--water (1/1)용매

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온도
50 °C

실험 절차

Methyl 3-(1-cyanophthalazin-6-yl)-4-methylbenzoate (120 mg, 396 μmol) was dissolved in THF/water (4:1) (3.96 mL) and LiOH (19 mg, 791 μmol) was added. The reaction mixture was stirred at 50° C. for 5.5 h, concentrated, and lyophilyzed under house vacuum. The reaction mixture was dissolved in DMF (791 μl) and HATU (301 mg, 791 μmol) and cyclopropylamine (277 μl, 3956 μmol) were added and the mixture was stirred at RT for 16 h. The mixture was diluted with 100 mL ethyl acetate, and partitioned with sodium bicarbonate (saturated, aqueous). The organic layers were washed 3×20 mL with sodium bicarbonate (saturated, aqueous), separated, dried over sodium sulfate, concentrated in vacuo, and purified by HPLC to give the title compound. MS (ES+): 347 (M+H)+.

후처리

  1. concentrationconcentrated
  2. dissolutionThe reaction mixture was dissolved in DMF (791 μl)
  3. stirringthe mixture was stirred at RT for 16 h
  4. custompartitioned with sodium bicarbonate (saturated, aqueous)
  5. washThe organic layers were washed 3×20 mL with sodium bicarbonate (saturated, aqueous)
  6. customseparated
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated in vacuo
  9. custompurified by HPLC

출처 및 근거

ORD 기록
ord-ca0fd3987ace4388b1ac43beffeef1bd
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07759337B2

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