Potassium Iodide → HCID 86734691, 화합물

HRID 329023

반응식

HRID 329023 반응식
[CH2:1]1[C@@H:11]2[C@H:5]([CH:6]=[CH:7][C:8]3[C:9]4[N:10]2[C:12]2[CH:21]=[CH:20][N:19]=[CH:18][C:13]=2[C:14]=4[CH2:15][CH2:16][CH:17]=3)[CH2:4][CH2:3][CH2:2]1.[I-].[K+].C(N(CC)CC)C.Cl[CH2:32][CH2:33][C:34]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)=[O:35]>CN(C=O)C>[CH2:1]1[CH:11]2[CH:5]([CH:6]=[CH:7][C:8]3[C:9]4[N:10]2[C:12]2[CH:21]=[CH:20][N:19]=[CH:18][C:13]=2[C:14]=4[CH2:15][CH2:16][CH:17]=3)[CH2:4][CH:3]([CH2:32][CH2:33][C:34]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[O:35])[CH2:2]1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 8471TriethylamineHCID 702953-ChloropropiophenoneHCID 86734686(+/-)-trans-1,2,3,4,4a,8,9,14a-Octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine

생성물 1

HCID 86734691HCID 86734691, 화합물수율 82.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

5.5 grams of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine, 3.6 grams of potassium iodide, 6.5 ml of triethylamine and 4.2 grams of β-chloropropiophenone were suspended in 100 ml DMF and heated to 60° C for 2 hours. The mixture was permitted to cool to room temperature, poured into 200 ml. of water and extracted with benzene. The benzene layer was washed with water, dried over potassium carbonate, filtered and evaporated to dryness in vacuo. The resulting oil was taken up in ether and converted to the hydrochloride salt as in Example 7, thus yielding 6.7 grams of the title compound, hydrochloride salt, m.p. 279° C (dec).

후처리

  1. temperatureto cool to room temperature
  2. additionpoured into 200 ml
  3. extractionof water and extracted with benzene
  4. washThe benzene layer was washed with water
  5. dry with materialdried over potassium carbonate
  6. filtrationfiltered
  7. customevaporated to dryness in vacuo

출처 및 근거

ORD 기록
ord-c8abf91e819e47d5af2509f284c7d117
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04018930

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