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Trifluoroacetic acid → Methyl 8-amino-5,6-dihydropyrazolo[5,1-a]isoquinoline-7-carboxylate

HRID 595117
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HRID 595117 반응식
C(O)(C(F)(F)F)=O.C(OC([N:15](C(OC(C)(C)C)=O)[C:16]1[CH:25]=[CH:24][C:23]2[C:22]3=[CH:26][CH:27]=[N:28][N:21]3[CH2:20][CH2:19][C:18]=2[C:17]=1[C:29]([O:31][CH3:32])=[O:30])=O)(C)(C)C.C(OC(NC1C=CC2C3=CC=NN3CCC=2C=1C(OC)=O)=O)(C)(C)C.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[NH2:15][C:16]1[CH:25]=[CH:24][C:23]2[C:22]3=[CH:26][CH:27]=[N:28][N:21]3[CH2:20][CH2:19][C:18]=2[C:17]=1[C:29]([O:31][CH3:32])=[O:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 70984431Methyl 8-tert-butoxycarbonylamino-5,6-dihydropyrazolo[5,1-a]isoquinoline-7-carboxylate2회HCID 70984636Methyl 8-[bis-(tert-butoxycarbonyl)amino]-5,6-dihydropyrazolo[5,1-a]isoquinoline-7-carboxylate

생성물 1

HCID 86712823Methyl 8-amino-5,6-dihydropyrazolo[5,1-a]isoquinoline-7-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

TFA (1 mL) was added to a mixture of methyl 8-[bis-(tert-butoxycarbonyl)amino]-5,6-dihydropyrazolo[5,1-a]isoquinoline-7-carboxylate and methyl 8-tert-butoxycarbonylamino-5,6-dihydropyrazolo[5,1-a]isoquinoline-7-carboxylate (Intermediate 23, 0.114 g) in DCM (2 mL) and the resultant mixture was stirred at room temperature for 1 hour. Saturated aqueous sodium bicarbonate solution was added and the mixture was stirred for 15 minutes, then extracted with DCM, dried (MgSO4) and filtered. The filtrate was concentrated in vacuo to give methyl 8-amino-5,6-dihydropyrazolo[5,1-a]isoquinoline-7-carboxylate (0.060 g) as a gum.

후처리

  1. extractionextracted with DCM
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-796da5ac38b9448cb0fc7528b7060789
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09242997B2

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