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

3-Chloropropyl(diethyl)amine → HCID 68143942, 화합물

HRID 1580802
노트
인쇄 미리보기

반응식

HRID 1580802 반응식
[O:1]=[C:2]1[O:7][C:6]2[CH:8]=[C:9]([C:12]([OH:14])=[O:13])[CH:10]=[CH:11][C:5]=2[C:4]2[CH:15]=[CH:16][C:17]([C:19]([OH:21])=[O:20])=[CH:18][C:3]1=2.[CH2:22]([N:24]([CH2:29][CH3:30])[CH2:25][CH2:26][CH2:27][Cl:28])[CH3:23]>[Cl-].C([N+](C)(C)C)C1C=CC=CC=1.C(O)(C)C>[ClH:28].[ClH:28].[O:1]=[C:2]1[O:7][C:6]2[CH:8]=[C:9]([C:12]([O:14][CH2:27][CH2:26][CH2:25][N:24]([CH2:29][CH3:30])[CH2:22][CH3:23])=[O:13])[CH:10]=[CH:11][C:5]=2[C:4]2[CH:15]=[CH:16][C:17]([C:19]([O:21][CH2:27][CH2:26][CH2:25][N:24]([CH2:29][CH3:30])[CH2:22][CH3:23])=[O:20])=[CH:18][C:3]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 669183-Chloropropyl(diethyl)amineHCID 21543589HCID 21543589, 화합물

생성물 1

HCID 68143942HCID 68143942, 화합물

시약·촉매·용매 2

HCID 5963Benzyltrimethylammonium chloride촉매HCID 3776Isopropanol용매

실험 절차

A mixture of 11.0 g (0.04 mole) of 6-oxo-6H-dibenzo [b,d]pyran-3,8-dicarboxylic acid, 18.0 g (0.12 mole) of γ-diethylaminopropyl chloride and 400 ml of isopropyl alcohol are stirred and heated to its reflux temperature. A catalytic amount of benzyltrimethylammonium chloride. 0.3 ml of a 60% aqueous solution, is added and the reaction mixture heated to reflux for an additional 24 hours. On cooling, the reaction mixture is filtered, and the residue washed with isopropyl alcohol. This product is dissolved in boiling ethanol, treated with charcoal, filtered and cooled to room temperature. After standing for 1 hour, the gelatinous precipitate which appears is filtered and the filtrate cooled to -20°C. The product which forms is filtered, washed with ethanol and again recrystallized from ethanol to yield the desired bis[3-(diethylamino)propyl] 6-oxo-6H-dibenzo[b,d]pyran-3,8-dicarboxylate dihydrochloride as a tan-colored solid, soluble in water and having a m.p. of 250°-1°C. (dec.) (placed in m.p. bath previously heated at 240° C.), λmax 294, and E1cm 1% 464.

후처리

  1. temperatureheated to its
  2. temperaturereflux temperature
  3. temperaturethe reaction mixture heated
  4. temperatureto reflux for an additional 24 hours
  5. temperatureOn cooling
  6. filtrationthe reaction mixture is filtered
  7. washthe residue washed with isopropyl alcohol
  8. dissolutionThis product is dissolved
  9. additiontreated with charcoal
  10. filtrationfiltered
  11. filtrationthe gelatinous precipitate which appears is filtered
  12. temperaturethe filtrate cooled to -20°C
  13. filtrationThe product which forms is filtered
  14. washwashed with ethanol
  15. customagain recrystallized from ethanol

출처 및 근거

ORD 기록
ord-de06c86d3ccf4a84bfa7f9b864882bdb
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03933893

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트