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Hydrochloric Acid → (2S)-5-(1,3,5Trimethyl-1H-pyrazol-4-yl)-1,2,3,4-tetrahydro-naphthalen-2-ylamine dihydrochloride

HRID 420783
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HRID 420783 반응식
[ClH:1].[CH3:2][N:3]1[C:7]([CH3:8])=[C:6]([C:9]2[CH:18]=[CH:17][CH:16]=[C:15]3[C:10]=2[CH2:11][CH2:12][C@H:13]([NH2:19])[CH2:14]3)[C:5]([CH3:20])=[N:4]1>CCOCC>[ClH:1].[ClH:1].[CH3:2][N:3]1[C:7]([CH3:8])=[C:6]([C:9]2[CH:18]=[CH:17][CH:16]=[C:15]3[C:10]=2[CH2:11][CH2:12][C@H:13]([NH2:19])[CH2:14]3)[C:5]([CH3:20])=[N:4]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 24989528(2S)-5-(1,3,5-Trimethyl-1H-pyrazol-4-yl)-1,2,3,4-tetrahydronaphthalen-2-amine

생성물 1

HCID 66658896(2S)-5-(1,3,5Trimethyl-1H-pyrazol-4-yl)-1,2,3,4-tetrahydro-naphthalen-2-ylamine dihydrochloride수율 91%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

HCl (0.42 mL, 4 M solution in dioxane, 1.688 mmol) was dropwise added to a suspension of (2S)-5-(1,3,5-Trimethyl-1H-pyrazol-4-yl)-1,2,3,4-tetrahydronaphthalen-2-amine (0.143 g, 0.563 mmol) in Et2O (5 mL). The reaction mixture was stirred at room temperature for 3 h and then the solvent was concentrated off. The resulting solid was suspended in Et2O (10 mL) and concentrated, in order to remove excess of HCl. This operation was repeated for three times, to give 0.150 g of the title product (Rf=0.2 (AcOEt/MeOH/Et3N 20:3:2), white solid, 91% yield).

후처리

  1. concentrationthe solvent was concentrated off
  2. concentrationconcentrated, in order
  3. customto remove excess of HCl

출처 및 근거

ORD 기록
ord-8691bf71b25c4f93bcd81b8956b1ec66
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08097641B2

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