홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Sodium Hydroxide → 3-(2-Chloro-10,11-dihydro-dibenzo[b,f]oxepin-10-yl)-8-methyl-3,8-diazabicyclo(3.2.1)octane monomaleate

HRID 1274076
노트
인쇄 미리보기

반응식

HRID 1274076 반응식
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH:9](Cl)[CH2:10][C:4]=2[CH:3]=1.Cl.Cl.[CH3:20][N:21]1[CH:26]2[CH2:27][CH2:28][CH:22]1[CH2:23][NH:24][CH2:25]2.[C:29](=[O:32])([OH:31])[O-].[Na+].[OH-:34].[Na+]>CCOCC.CN(C)C=O>[C:5]([OH:34])(=[O:6])/[CH:4]=[CH:10]\[C:29]([OH:31])=[O:32].[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH:9]([N:24]3[CH2:25][CH:26]4[N:21]([CH3:20])[CH:22]([CH2:28][CH2:27]4)[CH2:23]3)[CH2:10][C:4]=2[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 221201882,10-Dichloro-10,11-dihydro-dibenz[b,f]oxepinHCID 221201898-Methyl-3,8-diazabicyclo(3.2.1)octane dihydrochloride

생성물 1

HCID 867545003-(2-Chloro-10,11-dihydro-dibenzo[b,f]oxepin-10-yl)-8-methyl-3,8-diazabicyclo(3.2.1)octane monomaleate

시약·촉매·용매 2

HCID 3283
Diethyl Ether
용매
HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

A mixture of 2,10-Dichloro-10,11-dihydro-dibenz[b,f]oxepin (3.2 g), 8-Methyl-3,8-diazabicyclo(3.2.1)octane dihydrochloride (1.6 g), sodium bicarbonate (10 g), and dimethylformamide (40 mL) was stirred at 100° C. for 1 h. After cooling, the reaction mixture was poured onto water, made basic with NaOH and the products are extracted with ether. The ether layer was extracted with 3N HCl, the aqueous layer is basified and the basic product was reextracted with ether. After drying over magnesium sulfate the solvent was removed in vacua. The residue is dissolved in ethanol and 500 mg of maleic acid was added and the mixture was warmed until a clear solution is obtained. After dilution of this mixture with ether and cooling at -20° C. overnight, 3-(2-Chloro-10,11-dihydro-dibenzo[b,f]oxepin-10-yl)-8-methyl-3,8-diazabicyclo(3.2.1)octane monomaleate (Compound 1) melting at 169-170° C. was obtained as white crystals.

후처리

  1. temperatureAfter cooling
  2. additionthe reaction mixture was poured onto water
  3. extractionthe products are extracted with ether
  4. extractionThe ether layer was extracted with 3N HCl
  5. dry with materialAfter drying over magnesium sulfate the solvent
  6. customwas removed in vacua
  7. dissolutionThe residue is dissolved in ethanol
  8. addition500 mg of maleic acid was added
  9. temperaturethe mixture was warmed until a clear solution
  10. customis obtained

출처 및 근거

ORD 기록
ord-8172bec9b053490fbec03d37e81ed877
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06156751

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트