Water → HCID 57934072、化合物

HRID 1950007ノート

反応式

HRID 1950007 の反応式
[N:1]1([CH2:8][CH2:9][OH:10])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].Br[C:14]1[CH:19]=[CH:18][C:17]([Br:20])=[CH:16][N:15]=1.O>CN(C)C=O>[Br:20][C:17]1[CH:18]=[CH:19][C:14]([O:10][CH2:9][CH2:8][N:1]2[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)=[N:15][CH:16]=1

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 693532,5-DibromopyridineHCID 88615Hexahydro-1H-azepine-1-ethanol

生成物 1

HCID 57934072HCID 57934072、化合物収率 96.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2-azepan-1-ylethanol (5.0 g) in N,N-dimethylformamide (100 ml) was added 60% sodium hydride (1.5 g) under a nitrogen atmosphere, the solution was stirred for 1 hour at room temperature, 2,5-dibromopyridine (7.5 g) was then added thereto followed by stirring for 4.5 hours at room temperature. Water was added thereto followed by stirring, the solution was extracted with ethyl acetate, then sequentially washed with water and brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated in vacuo. The residue was purified by NH silica gel column chromatography (hexane-ethyl acetate system) to provide the title compound (9.1 g).

後処理

  1. stirringby stirring for 4.5 hours at room temperature
  2. stirringby stirring
  3. extractionthe solution was extracted with ethyl acetate
  4. washsequentially washed with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated in vacuo
  7. customThe residue was purified by NH silica gel column chromatography (hexane-ethyl acetate system)

出典と根拠

ORDレコード
ord-15710b4624304578b00b1cccade5a0e3
出典データセット
uspto-grants-2013_03
特許番号
US08399520B2

反応ノート

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