Sodium Iodide → HCID 12783765, 화합물

HRID 1979770노트

반응식

HRID 1979770 반응식
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH2:13][CH2:14][CH2:15]Cl)[CH:10]=2)[NH:5][C:4](=[O:17])[CH:3]=1.[I-].[Na+].[CH2:20]([CH:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(=O)([O-])O.[Na+]>C(N(CC)CC)C.CN(C)C=O.CC(C)=O>[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH2:13][CH2:14][CH2:15][N:30]3[CH2:31][CH2:32][CH:27]([CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)[CH2:28][CH2:29]3)[CH:10]=2)[NH:5][C:4](=[O:17])[CH:3]=1

참가 물질

8

반응물 4

HCID 5238Sodium IodideHCID 317384-BenzylpiperidineHCID 516892Sodium BicarbonateHCID 12899554HCID 12899554, 화합물

생성물 1

HCID 12783765HCID 12783765, 화합물수율 82%

시약·촉매·용매 3

HCID 180Acetone용매HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매

반응 조건

온도
50 °C

실험 절차

2.5 Grams of 4-methyl-6-(3-chloropropoxy)carbostyril, 1.8 g of sodium iodide were mixed with 50 ml of acetone and the mixture was stirred at 50° C. for 1 hour, then 50 ml of dimethylformamide was added and acetone was removed by distillation under a reduced pressure. To the residue thus obtained was added 1.5 g of triethylamine and 1.6 g of 4-benzylpiperidine and the mixture was heated at 70°-80° C. for 7 hours under stirring condition. The reaction mixture was then concentrated under a reduced pressure to dryness and to the residue thus obtained was added 60 ml of a 5%-sodium hydrogencarbonate aqueous solution and stirred to obtain the insoluble matters. The insoluble matters were collected by filtration, washed with water and then recrystallized from methanol to obtain 3.2 g (yield: 82%) of 4-methyl-6-[3-(4-benzyl-1-piperidyl)propoxy]-carbostyril as in the form of yellowish prism-like crystals. Melting point: 177°-178° C.

후처리

  1. customacetone was removed by distillation under a reduced pressure
  2. customTo the residue thus obtained
  3. temperaturethe mixture was heated at 70°-80° C. for 7 hours
  4. stirringunder stirring condition
  5. concentrationThe reaction mixture was then concentrated under a reduced pressure to dryness and to the residue
  6. customthus obtained
  7. stirringstirred
  8. customto obtain the insoluble matters
  9. filtrationThe insoluble matters were collected by filtration
  10. washwashed with water
  11. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-33d37c4bdd1e42c1af5b43130fa3024f
출처 데이터셋
uspto-grants-1984_11
특허 번호
US04482560

반응 노트

불러오는 중…