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Sodium Iodide → HCID 12899539, 화합물

HRID 621561
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HRID 621561 반응식
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:7]=1[CH2:8][CH2:9][C:10](=[O:16])[NH:11]2.[I-].[Na+].[CH2:19]([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(=O)([O-])O.[Na+]>C(N(CC)CC)C.CN(C)C=O.CC(C)=O>[CH2:19]([N:26]1[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:15]=[CH:14][CH:13]=[C:12]3[C:7]=2[CH2:8][CH2:9][C:10](=[O:16])[NH:11]3)[CH2:28][CH2:27]1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 5238Sodium IodideHCID 759941-BenzylpiperazineHCID 516892Sodium BicarbonateHCID 12899139HCID 12899139, 화합물

생성물 1

HCID 12899539HCID 12899539, 화합물수율 84.2%

시약·촉매·용매 3

HCID 180Acetone용매
HCID 6228
Dimethylformamide
용매
HCID 8471Triethylamine용매

실험 절차

24 grams of 5-(3-chloropropoxy)-3,4-dihydrocarbostyril and 17 g of sodium iodide are mixed with 300 ml of acetone and heated for 3 hours under refluxing conditions. Then, 300 ml of dimethylformamide, 12 g of triethylamine and 18 g of 4-benzylpiperazine are added thereto and the reaction is carried out at 60°-70° C. for 7 hours under stirring conditions. The reactions mixture is concentrated under a reduced pressure to obtain a viscous liquid, then 300 ml of 3% sodium hydrogencarbonate aqueous solution are added. The organic layer is extracted with chloroform and washed with water. After drying the chloroform layer, chloroform is removed by distillation. The residue thus obtained is washed with ether and recrystallized from methanol to obtain 32 g (yield: 84%) of 5-[3-(4-benzylpiperazinyl)propoxy]-3,4-dihydrocarbostyril in the form of colorless needle-like crystals with a melting point of 157°-159° C.

후처리

  1. temperatureheated for 3 hours under refluxing conditions
  2. concentrationThe reactions mixture is concentrated under a reduced pressure
  3. customto obtain a viscous liquid
  4. extractionThe organic layer is extracted with chloroform
  5. washwashed with water
  6. dry with materialAfter drying the chloroform layer, chloroform
  7. customis removed by distillation
  8. customThe residue thus obtained
  9. washis washed with ether
  10. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-7c43a7bdc2c4467aab4cc9d06094cd98
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04824840

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