1-Bromo-3-chloropropane → 1-(4-Chlorobenzyl)-4-(3-chloropropyl)homopiperazine

HRID 3844ノート

反応式

HRID 3844 の反応式
Br[CH2:2][CH2:3][CH2:4][Cl:5].[Cl:6][C:7]1[CH:20]=[CH:19][C:10]([CH2:11][N:12]2[CH2:18][CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[CH:9][CH:8]=1.[OH-].[K+]>CS(C)=O>[Cl:6][C:7]1[CH:20]=[CH:19][C:10]([CH2:11][N:12]2[CH2:18][CH2:17][CH2:16][N:15]([CH2:2][CH2:3][CH2:4][Cl:5])[CH2:14][CH2:13]2)=[CH:9][CH:8]=1

参加物

5

反応物 3

HCID 80061-Bromo-3-chloropropaneHCID 14797Potassium HydroxideHCID 156343771-[(4-Chlorophenyl)methyl]-1,4-diazepane

生成物 1

HCID 201531881-(4-Chlorobenzyl)-4-(3-chloropropyl)homopiperazine収率 42%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

15.7 g of 1-bromo-3-chloropropane were added to a cooled solution of 15.0 g of 1-(4-chlorobenzyl)homopiperazine and 12.0 g of potassium hydroxide in 50 ml of dimethyl sulfoxide. The mixture was stirred at 5°-10° C. for one hour, and then an additional 30 minutes at room temperature. After the addition of ice water, the product was extracted with ether, and the extract was dried (magnesium sulfate) and concentrated in vacuo. Final purification was effected on a silica gel column (methylene chloride:methanol, 9:1), and the solvent was removed in vacuo to give 8.4 g (42% of theory) of 1-(4-chlorobenzyl)-4-(3-chloropropyl)homopiperazine as an oil.

後処理

  1. customan additional 30 minutes
  2. customat room temperature
  3. extractionthe product was extracted with ether
  4. dry with materialthe extract was dried (magnesium sulfate)
  5. concentrationconcentrated in vacuo
  6. customFinal purification
  7. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-0956ad0caa5041f28456e5e148238e1e
出典データセット
uspto-grants-1988_02
特許番号
US04722926

反応ノート

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