2-Chlorobenzyl chloride → HCID 57682471, 화합물

HRID 493904노트

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HRID 493904 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 57682471HCID 57682471, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-65e182d9882d4f53bd2d9884fc923037
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538104B2

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