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Methanol → 4-Phenoxy-2-pyridinemethanamine

HRID 2080044
ノート
印刷プレビュー

反応式

HRID 2080044 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[O:7]([C:14]1[CH:19]=[CH:18][N:17]=[C:16]([C:20]#[N:21])[CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.CO.[Cl-].[NH4+]>O1CCCC1.O>[O:7]([C:14]1[CH:19]=[CH:18][N:17]=[C:16]([CH2:20][NH2:21])[CH:15]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 887MethanolHCID 25517Ammonium ChlorideHCID 21226445Aluminium lithium hydrideHCID 23130778HCID 23130778、化合物

生成物 1

HCID 231304504-Phenoxy-2-pyridinemethanamine収率 48%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

Next, to a solution of lithium aluminum hydride (725 mg, 19.1 mmol) in tetrahydrofuran (6.0 mL) was portionwise added a solution of the resulting 4-phenoxy-pyridine-2-carbonitrile (1.5 g, 7.65 mmol) in tetrahydrofuran (3 mL) on an ice bath, and the solution was stirred at room temperature for 15 hours. A mixture solvent of methanol and water (9:1) was added to the reaction solution, an aqueous solution of saturated ammonium chloride was further added, the solution was extracted with ethyl acetate, dried over anhydrous magnesium sulfate, then, the solvent was evaporated to obtain the title compound (730 mg, 48%) as a pale brown oil. This was used in the next reaction without further purification.

後処理

  1. extractionthe solution was extracted with ethyl acetate
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-1bb7d980371946e8a233d29f8ec17b72
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932272B2

反応ノート

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