Potassium Iodide → HCID 20379982, 화합물

HRID 1658670노트

반응식

HRID 1658670 반응식
[C:1]1([C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:21][CH2:22][CH2:23][C:24]([C:26]1[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=1)=[O:25].C(=O)(O)[O-].[K+].[I-].[K+]>C1(C)C=CC=CC=1.C(OCC)(=O)C>[F:32][C:29]1[CH:28]=[CH:27][C:26]([C:24](=[O:25])[CH2:23][CH2:22][CH2:21][N:11]2[CH2:10][CH2:9][C:8](=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:13][CH2:12]2)=[CH:31][CH:30]=1

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 197503-(4-Fluorobenzoyl)propyl chlorideHCID 516893Potassium BicarbonateHCID 27625334-(Diphenylmethylene)piperidine

생성물 1

HCID 20379982HCID 20379982, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 99.9 g (0.4 mole) of 4-diphenylmethylenepiperidine, 88 g (0.44 mole) of 4-chloro-4'-fluorobutyrophenone, 64.0 g (0.64 mole) of potassium bicarbonate and a small amount of potassium iodide in 1500 ml of toluene was refluxed for 5 days. The reaction mixture was filtered, and the filtrate was concentrated at reduced pressure leaving a residue which was dissolved in about 800 ml of ethyl acetate. This solution was concentrated to about 500 ml and allowed to stand for one day. The resulting precipitate was recrystallized from methanolethyl acetate, made basic with sodium hydroxide solution, water washed, and the product recrystallized from 75°-90° petroleum ether to give the title compound, M.P. 111°-114° C.

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated at reduced pressure
  3. customleaving a residue which
  4. concentrationThis solution was concentrated to about 500 ml
  5. customThe resulting precipitate was recrystallized from methanolethyl acetate
  6. washwashed
  7. customthe product recrystallized from 75°-90° petroleum ether

출처 및 근거

ORD 기록
ord-9035fe5031dd4796aecb340fc9727f1d
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03965257

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