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

HRID 595117
ノート
印刷プレビュー

反応式

HRID 595117 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 70984431Methyl 8-tert-butoxycarbonylamino-5,6-dihydropyrazolo[5,1-a]isoquinoline-7-carboxylate2 回HCID 70984636Methyl 8-[bis-(tert-butoxycarbonyl)amino]-5,6-dihydropyrazolo[5,1-a]isoquinoline-7-carboxylate

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-796da5ac38b9448cb0fc7528b7060789
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09242997B2

反応ノート

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