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

HRID 2290899

반응식

HRID 2290899 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 201531881-(4-Chlorobenzyl)-4-(3-chloropropyl)homopiperazine수율 42%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5ccc732570e64ea09e94a3855cb22b8d
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04618677

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