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Diisopropylethylamine → HCID 44227504, 화합물

HRID 1914572
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HRID 1914572 반응식
[NH:1]1[CH:5]=[C:4]([C:6]2[S:10][CH:9]=[C:8]([C:11]([OH:13])=O)[CH:7]=2)[CH:3]=[N:2]1.Cl.[CH3:15][C:16]1([CH3:22])[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1.CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C>[CH3:15][C:16]1([CH3:22])[CH2:21][CH2:20][N:19]([C:11]([C:8]2[CH:7]=[C:6]([C:4]3[CH:5]=[N:1][NH:2][CH:3]=3)[S:10][CH:9]=2)=[O:13])[CH2:18][CH2:17]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 222529024,4-Dimethylpiperidinium chlorideHCID 581101935-(1H-Pyrazol-4-YL)thiophene-3-carboxylic acid

생성물 1

HCID 44227504HCID 44227504, 화합물수율 55.8%

시약·촉매·용매

1
HCID 6228Dimethylformamide용매

실험 절차

5-(1H-Pyrazol-4-yl)-thiophene-3-carboxylic acid (0.075 g, 0.39 mmol) and 4,4-dimethylpiperidine hydrochloride (0.087 g, 0.58 mmol) were dissolved in DMF (3 mL) then DIPEA (0.2 g, 1.55 mmol) and HATU (0.175 g, 1.55 mmol) were added and the reaction mixture was stirred at room temperature overnight. The solvent was removed by evaporation then the residue was dissolved in DCM and washed with aqueous sodium hydrogen carbonate solution. The organics were dried by evaporation. The crude material was purified by HPLC, eluting with 5%-98% acetonitrile in water (0.1% formic acid) over 20 minutes. The fractions containing the desired product were freeze-dried to give the title compound (0.063 g). LCMS m/z 290.18 [M+H]+ R.T.=8.74 min (Analytical Method 2).

후처리

  1. customThe solvent was removed by evaporation
  2. dissolutionthe residue was dissolved in DCM
  3. washwashed with aqueous sodium hydrogen carbonate solution
  4. customThe organics were dried by evaporation
  5. customThe crude material was purified by HPLC
  6. washeluting with 5%-98% acetonitrile in water (0.1% formic acid) over 20 minutes
  7. additionThe fractions containing the desired product
  8. customwere freeze-dried

출처 및 근거

ORD 기록
ord-4df150d594a84c34b9a27bbde1361eb4
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08614209B2

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