Potassium Iodide → HCID 20379982、化合物

HRID 1448501ノート

反応式

HRID 1448501 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 20379982HCID 20379982、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 99.9 g (0.4 mole) of 4-(diphenylmethylene)piperidine, 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 methanol-ethyl acetate, made basic with sodium hydroxide solution, water washed, and the product recrystallized from petroleum-ether to give the title compound, M.P. 111°-114° C.

後処理

  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 methanol-ethyl acetate
  6. washwashed
  7. customthe product recrystallized from petroleum-ether

出典と根拠

ORDレコード
ord-29d5ed83c1b149c987048b6a6ee6d98b
出典データセット
uspto-grants-1979_12
特許番号
US04180583

反応ノート

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