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

HRID 536595
ノート
印刷プレビュー

反応式

HRID 536595 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 66848215(+/-)Tert-butyl 7-(((6-methylpyridin-2-yl)amino)methyl)-8-azaspiro[4.5]decane-8-carboxylate2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

(±)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.

後処理

  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

出典と根拠

ORDレコード
ord-4bec20d37dd04371a148673dc83774ca
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08859608B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート