2-Chlorobenzyl chloride → HCID 57682471、化合物

HRID 888756ノート

反応式

HRID 888756 の反応式
[N:1]12[CH2:9][CH2:8][CH2:7][C:6]1=[N:5][CH2:4][CH2:3][CH2:2]2.[Cl:10][C:11]1[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=1[CH2:13]Cl.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>O1CCCC1.O>[Cl:10][C:11]1[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=1[CH2:13][N:5]1[CH:6]2[N:1]([CH2:9][CH2:8][CH2:7]2)[CH2:2][CH2:3][CH2:4]1

参加物

7

反応物 4

HCID 119062-Chlorobenzyl chlorideHCID 14798Sodium HydroxideHCID 763491,5-Diazabicyclo(4.3.0)non-5-eneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 57682471HCID 57682471、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

In a 250 ml three-necked flask, 5 g (0.04 mol) of 1,5-diazabicyclo[4.3.0]non-5-ene are dissolved in 100 ml of tetrahydrofuran, and at room temperature 6.48 g (0.04 mol) of 2-chlorobenzyl chloride are slowly added with stirring. A colourless suspension is formed which is stirred overnight. The suspension is then filtered, the salt isolated by filtration is washed, and the washed salt is suspended in 100 ml of tetrahydrofuran. Added to this suspension in portions is 0.76 g (0.02 mol) of lithium aluminium hydride. After the end of the addition, the reaction mixture is stirred at room temperature overnight. It is then cooled to 0° C. and, dropwise, 0.8 g of water, then 0.8 g of 10% strength sodium hydroxide solution and a further 2.4 g of water are added. The resulting suspension is stirred at room temperature for 30 minutes and then filtered. The filter cake is washed with tetrahydrofuran and the combined organic phases are dried and concentrated on a rotary evaporator. This gives 7.15 g of 5-(2-chlorobenzyl)-1,5-diazabicyclo[4.3.0]nonane as a colourless oil.

後処理

  1. customA colourless suspension is formed which
  2. stirringis stirred overnight
  3. filtrationThe suspension is then filtered
  4. customthe salt isolated by filtration
  5. washis washed
  6. additionAdded to this suspension in portions
  7. additionAfter the end of the addition
  8. stirringthe reaction mixture is stirred at room temperature overnight
  9. stirringThe resulting suspension is stirred at room temperature for 30 minutes
  10. filtrationfiltered
  11. washThe filter cake is washed with tetrahydrofuran
  12. customthe combined organic phases are dried
  13. concentrationconcentrated on a rotary evaporator

出典と根拠

ORDレコード
ord-69c5a7356392466d8a9f203a4abafb86
出典データセット
uspto-grants-2012_08
特許番号
US08252784B2

反応ノート

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