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Hydrochloric Acid → N-Cyclopropylmethyl-N-[7-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-2-(methoxymethyl)pyrazolo[1,5-a]pyridin-3-yl]amine

HRID 347854
ノート
印刷プレビュー

反応式

HRID 347854 の反応式
[CH:1]1([CH2:4][N:5]([C:13]2[C:14]([CH2:35][O:36][CH3:37])=[N:15][N:16]3[C:21]([C:22]4[C:27]([O:28][CH3:29])=[CH:26][C:25]([CH2:30][O:31][CH3:32])=[CH:24][C:23]=4[O:33][CH3:34])=[CH:20][CH:19]=[CH:18][C:17]=23)C(=O)OC(C)(C)C)[CH2:3][CH2:2]1.Cl.[OH-].[Na+]>C(OCC)(=O)C>[CH:1]1([CH2:4][NH:5][C:13]2[C:14]([CH2:35][O:36][CH3:37])=[N:15][N:16]3[C:21]([C:22]4[C:23]([O:33][CH3:34])=[CH:24][C:25]([CH2:30][O:31][CH3:32])=[CH:26][C:27]=4[O:28][CH3:29])=[CH:20][CH:19]=[CH:18][C:17]=23)[CH2:3][CH2:2]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

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21084194tert-butyl N-cyclopropylmethyl-N-[7-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-2-(methoxymethyl)pyrazolo[1,5-a]pyridin-3-yl]carbamate

生成物 1

HCID 21084165N-Cyclopropylmethyl-N-[7-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-2-(methoxymethyl)pyrazolo[1,5-a]pyridin-3-yl]amine

試薬・触媒・溶媒 1

HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
40 °C

実験手順

The obtained tert-butyl N-cyclopropylmethyl-N-[7-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-2-(methoxymethyl)pyrazolo[1,5-a]pyridin-3-yl]carbamate was dissolved in ethyl acetate (5 mL) without purification, and then 4N hydrochloric acid (ethyl acetate solution; 10 mL) was added thereto and the reaction mixture was stirred for 30 minutes at 40° C. The reaction mixture was neutralized with a 5N aqueous sodium hydroxide solution while cooling with ice, and then the reaction mixture was extracted with ethyl acetate and the organic extract was washed with water and brine. The organic extract was dried over anhydrous magnesium sulfate and filtered, the solvent was evaporated under reduced pressure, the residue was purified by silica gel column chromatography and the title compound (95 mg) was obtained as a yellow oil from the n-hexane:ethyl acetate (2:3) fraction.

後処理

  1. temperaturewhile cooling with ice
  2. extractionthe reaction mixture was extracted with ethyl acetate
  3. extractionthe organic extract
  4. washwas washed with water and brine
  5. extractionThe organic extract
  6. dry with materialwas dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent was evaporated under reduced pressure
  9. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-c8ab5c0ba1d2496f9b9e5f3d5b23e41d
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07176216B2

反応ノート

読み込み中…

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