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Trifluoroacetic acid → N-(6-methyl-2-pyridinyl)-8-azaspiro[4.5]decane-7-methanamine

HRID 536595
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HRID 536595 반응식
[CH3:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH:10]2[N:19](C(OC(C)(C)C)=O)[CH2:18][CH2:17][C:12]3([CH2:16][CH2:15][CH2:14][CH2:13]3)[CH2:11]2)[CH:5]=[CH:4][CH:3]=1.FC(F)(F)C(O)=O>ClCCl>[CH2:13]1[C:12]2([CH2:17][CH2:18][NH:19][CH:10]([CH2:9][NH:8][C:6]3[CH:5]=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=3)[CH2:11]2)[CH2:16][CH2:15][CH2:14]1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66848215(+/-)Tert-butyl 7-(((6-methylpyridin-2-yl)amino)methyl)-8-azaspiro[4.5]decane-8-carboxylate2회

생성물 1

HCID 67497134N-(6-methyl-2-pyridinyl)-8-azaspiro[4.5]decane-7-methanamine수율 95.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

(±)tert-butyl 7-(((6-methylpyridin-2-yl)amino)methyl)-8-azaspiro[4.5]decane-8-carboxylate (intermediate 73, 1.3 g, 3.62 mmol) was dissolved in dichloromethane (10 ml) and cooled to 0° C., then trifluoroacetic acid (30 ml) was added. After 1 hour at 0° C. and 2 hours at room temperature the solution was evaporated, the residue re-dissolved in dichloromethane was washed with saturated NaHCO3 aqueous solution. The organic layers were dried (Na2SO4) and concentrated under vacuum to obtain 900 mg of the title compound.

후처리

  1. custom2 hours at room temperature the solution was evaporated
  2. dissolutionthe residue re-dissolved in dichloromethane
  3. washwas washed with saturated NaHCO3 aqueous solution
  4. dry with materialThe organic layers were dried (Na2SO4)
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-4bec20d37dd04371a148673dc83774ca
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859608B2

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