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Potassium Iodide → 8-[4,4-Bis(p-fluorophenyl)cyclohexyl]-1-(p-fluorophenyl)-1,3,8-triazaspiro[4.5]decan-4-one

HRID 616996
ノート
印刷プレビュー

反応式

HRID 616996 の反応式
S(O[CH:6]1[CH2:11][CH2:10][C:9]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH2:8][CH2:7]1)(=O)(=O)C.[F:26][C:27]1[CH:32]=[CH:31][C:30]([N:33]2[C:37]3([CH2:42][CH2:41][NH:40][CH2:39][CH2:38]3)[C:36](=[O:43])[NH:35][CH2:34]2)=[CH:29][CH:28]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].C(OC(C)C)(C)C>O.CN(C)C=O>[F:25][C:22]1[CH:23]=[CH:24][C:19]([C:9]2([C:12]3[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=3)[CH2:8][CH2:7][CH:6]([N:40]3[CH2:39][CH2:38][C:37]4([N:33]([C:30]5[CH:29]=[CH:28][C:27]([F:26])=[CH:32][CH:31]=5)[CH2:34][NH:35][C:36]4=[O:43])[CH2:42][CH2:41]3)[CH2:11][CH2:10]2)=[CH:20][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 4875Potassium IodideHCID 7914Diisopropyl EtherHCID 11430Potassium CarbonateHCID 939151-(4-Fluorophenyl)-1,3,8-triazaspiro(4.5)decan-4-oneHCID 203668854,4-Bis(p-fluorophenyl)cyclohexyl mesylate

生成物 1

HCID 133641518-[4,4-Bis(p-fluorophenyl)cyclohexyl]-1-(p-fluorophenyl)-1,3,8-triazaspiro[4.5]decan-4-one

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 16 g of 4,4-bis(p-fluorophenyl)cyclohexyl mesylate, 10 g of 1-(p-fluorophenyl)-1,3,8-triazaspiro[4.5]decan-4-one (m.p. 234°-234.5° C), 6.1 g of potassium carbonate, 7.3 g of potassium iodide and 100 ml of dimethylformamide is stirred at 70°-80° C for 50 hours. The reaction mixture is poured into water, isopropyl ether is added to the aqueous mixture, and the resulting mixture is stirred for some time. The precipitated crystals are collected by filtration and dissolved in a mixture of chloroform and methanol (9:1). The solvent is removed to some degree and cooled in an ice bath. The precipitated crystals are collected by filtration and purified in the same manner to give 8-[4,4-bis(p-fluorophenyl)cyclohexyl]-1-(p-fluorophenyl)-1,3,8-triazaspiro[4.5]decan-4-one as white crystals, melting at 237°-240° C.

後処理

  1. additionis added to the aqueous mixture
  2. stirringthe resulting mixture is stirred for some time
  3. filtrationThe precipitated crystals are collected by filtration
  4. dissolutiondissolved in a mixture of chloroform and methanol (9:1)
  5. customThe solvent is removed to some degree
  6. temperaturecooled in an ice bath
  7. filtrationThe precipitated crystals are collected by filtration
  8. custompurified in the same manner

出典と根拠

ORDレコード
ord-ff2233a8833a477bb5ba29a4969d5d31
出典データセット
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04076821

反応ノート

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