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Trifluoroacetic acid → HCID 46199246, 화합물

HRID 1959348
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HRID 1959348 반응식
C(OC([N:8](C(OC(C)(C)C)=O)[C:9]1[C:10]([C:16]2[N:20](C(OC(C)(C)C)=O)[C:19]3[CH:28]=[C:29]([CH3:32])[CH:30]=[CH:31][C:18]=3[N:17]=2)=[N:11][C:12](Br)=[CH:13][N:14]=1)=O)(C)(C)C.[NH:40]1[CH2:45][CH2:44]S[CH2:42][CH2:41]1.C1C=C(Cl)C=C(C(OO)=O)C=1.C(O)(C(F)(F)F)=O.C([O-])([O-])=O.[Na+].[Na+].[O-:70][S:71]([O-:74])(=S)=O.[Na+].[Na+]>CN(C=O)C.CCOC(C)=O>[O:70]=[S:71]1(=[O:74])[CH2:44][CH2:45][N:40]([C:12]2[N:11]=[C:10]([C:16]3[NH:20][C:19]4[CH:28]=[C:29]([CH3:32])[CH:30]=[CH:31][C:18]=4[N:17]=3)[C:9]([NH2:8])=[N:14][CH:13]=2)[CH2:41][CH2:42]1
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참가 물질

8

반응물 5

HCID 6422Trifluoroacetic acidHCID 67164ThiomorpholineHCID 70297m-Chloroperbenzoic acidHCID 20482104HCID 20482104, 화합물HCID 86661948HCID 86661948, 화합물

생성물 1

HCID 46199246HCID 46199246, 화합물수율 31%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
60 °C

실험 절차

A solution of tert-butyl 2-[3-[bis(tert-butoxycarbonyl)amino]-6-bromo-pyrazin-2-yl]-6-methyl-benzimidazole-1-carboxylate (70 mg, 0.1158 mmol) in DMF (2 mL) was treated with thiomorpholine (59.74 mg, 0.5790 mmol) and heated to 60° C. for 3 hours. The mixture was then diluted with EtOAc, washed with water, brine, dried (MgSO4) and concentrated in vacuo. The residue was dissolved in DCM (10 mL), treated with mCPBA (59.95 mg, 0.3474 mmol) and stirred at RT for 1 hour. After washing with a 1:1 Na2CO3/Na2S2O3 solution, TFA (264.1 mg, 178.4 μL, 2.316 mmol) was added and the mixture stirred at RT for 1 hour. This was concentrated in vacuo and the resultant residue was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 uM, 100A column, gradient 10%-95% B (solvent A: 0.05% TFA in water, solvent B: CH3CN) over 16 minutes at 25 mL/min]. The fractions were collected and freeze-dried to give the title compound (13.1 mg, 31% Yield).

후처리

  1. washwashed with water, brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in DCM (10 mL)
  5. additionwas added
  6. stirringthe mixture stirred at RT for 1 hour
  7. concentrationThis was concentrated in vacuo
  8. customthe resultant residue was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 uM, 100A column, gradient 10%-95% B (solvent A: 0.05% TFA in water, solvent B: CH3CN) over 16 minutes at 25 mL/min]
  9. customThe fractions were collected
  10. customfreeze-dried

출처 및 근거

ORD 기록
ord-c62c62b36c5c479d86d1642890072497
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08410112B2

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