Potassium Iodide → HCID 86734690, 화합물

HRID 329022

반응식

HRID 329022 반응식
[I-].[K+].C([N:5]([CH2:8]C)[CH2:6][CH3:7])C.[CH:10]1[N:18]2[C:19]3[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=3[CH:21]=[CH:22][C:16]3=[C:17]2[C:12](=[CH:13][CH:14]=[CH:15]3)[CH:11]=1.C1O[C:30]([CH2:32][CH2:33][CH2:34]Cl)([CH3:31])[O:29]C1>O.CN(C=O)C>[CH2:26]1[CH:19]2[CH:20]([CH:21]=[CH:22][C:16]3[C:17]4[N:18]2[C:10]2[CH:7]=[CH:6][N:5]=[CH:8][C:11]=2[C:12]=4[CH2:13][CH2:14][CH:15]=3)[CH2:23][CH:24]([CH2:34][CH2:33][CH2:32][C:30](=[O:29])[CH3:31])[CH2:25]1

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 8471TriethylamineHCID 800792-(3-Chloropropyl)-2-methyl-1,3-dioxolaneHCID 12752824HCID 12752824, 화합물

생성물 1

HCID 86734690HCID 86734690, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
62 °C

실험 절차

3.6 grams of potassium iodide and 12 ml. of triethylamine were added to a solution of 5.5 grams of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]=indolo[1,7-ab][1]benzazepine in 50 ml. DMF, followed by addition of 3.7 grams of 5-chloro-2-pentanone ethylene ketal. The mixture was heated at approximately 62° C for 20 hours. The mixture was then poured into water, extracted with benzene, and chromatographed through basic alumina to eliminate remaining benzazepine starting material. The resulting ketal was dissolved in ether. HCl gas was bubbled through this solution to precipitate the hydrochloride salt of the title compound. Recrystallization from ethanol yielded 350 mg. of the title compound, hydrochloride salt, m.p. 258°-259° C(dec).

후처리

  1. extractionextracted with benzene
  2. customchromatographed through basic alumina
  3. dissolutionThe resulting ketal was dissolved in ether
  4. customHCl gas was bubbled through this solution
  5. customto precipitate the hydrochloride salt of the title compound
  6. customRecrystallization from ethanol
  7. customyielded 350 mg

출처 및 근거

ORD 기록
ord-eefc34aa945b440da2ec42f1a254114a
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04018930

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