Potassium Iodide → HCID 21528589, 화합물

HRID 1658666노트

반응식

HRID 1658666 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:32])[CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH:15]([C:18]([OH:31])([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:14][CH2:13]2)=[CH:4][CH:3]=1.Cl.FC1C=CC(C(=O)CCC[N:45]2[CH2:50][CH2:49][CH:48](C(O)(C3C=CC=CC=3)C3C=CC=CC=3)[CH2:47][CH2:46]2)=CC=1.[I-].[K+]>N1CCCCC1>[OH:31][C:18]([CH:15]1[CH2:16][CH2:17][N:12]([CH2:11][CH2:10][CH2:9][C:8]([C:5]2[CH:6]=[CH:7][C:2]([N:45]3[CH2:50][CH2:49][CH2:48][CH2:47][CH2:46]3)=[CH:3][CH:4]=2)=[O:32])[CH2:13][CH2:14]1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 2061821-Butanone, 1-(4-fluorophenyl)-4-(4-(hydroxydiphenylmethyl)-1-piperidinyl)-, hydrochlorideHCID 206183HCID 206183, 화합물

생성물 1

HCID 21528589HCID 21528589, 화합물

시약·촉매·용매 1

HCID 8082Piperidine용매

실험 절차

A mixture of 15 g (0.035 mole) of 4'-fluoro-4-[4-(α-hydroxy-α-phenylbenzyl)piperidino]butyrophenone, the free base of the compound of Example 1, and a small amount of potassium iodide in 100 ml of piperidine was refluxed for 22 hours. The unreacted piperidine was removed under vacuum, and the remaining residue was triturated with water, the water decanted, and the residue dissolved in methanol and added to a large amount of water. The resulting precipitate was dissolved in a large volume of ether, dried over magnesium sulfate, treated with charcoal and filtered. The filtrate was concentrated to a 50 ml volume and cooled, yielding a product which was recrystallized from ether to give the title compound, M.P. 137.5°-139° C.

후처리

  1. customThe unreacted piperidine was removed under vacuum
  2. customthe remaining residue was triturated with water
  3. customthe water decanted
  4. dissolutionthe residue dissolved in methanol
  5. additionadded to a large amount of water
  6. dissolutionThe resulting precipitate was dissolved in a large volume of ether
  7. dry with materialdried over magnesium sulfate
  8. additiontreated with charcoal
  9. filtrationfiltered
  10. concentrationThe filtrate was concentrated to a 50 ml volume
  11. temperaturecooled
  12. customyielding a product which
  13. customwas recrystallized from ether

출처 및 근거

ORD 기록
ord-a5257876677443108786e040a31e448f
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03965257

반응 노트

불러오는 중…