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4-(Trifluoromethyl)benzylamine → 8-(1-Benzyl-1H-pyrazol-4-yl)-2-methylamino-1-propyl-1,7-dihydro-purin-6-one

HRID 536022
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HRID 536022 반응식
[CH2:1]([N:8]1[CH:12]=[C:11]([C:13]2[NH:21][C:20]3[C:19](=[O:22])[N:18]([CH2:23][CH2:24][CH3:25])[C:17](Cl)=[N:16][C:15]=3[N:14]=2)[CH:10]=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:27]([N:30](C(C)C)CC)(C)C.FC(F)(F)C1C=CC(CN)=CC=1>CN1C(=O)CCC1>[CH2:1]([N:8]1[CH:12]=[C:11]([C:13]2[NH:21][C:20]3[C:19](=[O:22])[N:18]([CH2:23][CH2:24][CH3:25])[C:17]([NH:30][CH3:27])=[N:16][C:15]=3[N:14]=2)[CH:10]=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

5

반응물 3

HCID 768044-(Trifluoromethyl)benzylamineHCID 81531DiisopropylethylamineHCID 469130818-(1-benzyl-1H-pyrazol-4-yl)-2-chloro-1-propyl-1,7-dihydro-purin-6-one

생성물 1

HCID 469132718-(1-Benzyl-1H-pyrazol-4-yl)-2-methylamino-1-propyl-1,7-dihydro-purin-6-one수율 44.5%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone
용매

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온도
110 °C

실험 절차

To a solution of 8-(1-Benzyl-1H-pyrazol-4-yl)-2-chloro-1-propyl-1,7-dihydro-purin-6-one (0.05 g, 0.136 mmol) in NMP (1 ml) under argon was added Diisopropyl ethyl amine (0.035 g, 0.27 mmol) and 4-Trifluoromethyl-benzylamine (0.035 g, 0.203 mmol). The reaction mixture was heated at 110° C. for overnight. The reaction mixture concentrated under reduced pressure. The residue was obtained was purified by preparative HPLC to obtain 8-(1-Benzyl-1H-pyrazol-4-yl)-2-methylamino-1-propyl-1,7-dihydro-purin-6-one (0.022 g, 32%) as a white solid.

후처리

  1. concentrationThe reaction mixture concentrated under reduced pressure
  2. customThe residue was obtained
  3. customwas purified by preparative HPLC

출처 및 근거

ORD 기록
ord-544ec8b6a1d640a2a9c72ba3ef492704
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859566B2

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