Potassium Iodide → HCID 86734691、化合物

HRID 329023

反応式

HRID 329023 の反応式
[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

参加物

6

反応物 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

生成物 1

HCID 86734691HCID 86734691、化合物収率 82.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c8abf91e819e47d5af2509f284c7d117
出典データセット
uspto-grants-1977_04
特許番号
US04018930

関連ノート

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