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Sodium Iodide → 3-[4-[4-(4-Fluorobenzoyl)piperidin-1-yl]-butyl]thieno[3,4-d]pyrimidine-2,4-dione

HRID 2165208
ノート
印刷プレビュー

反応式

HRID 2165208 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][NH:6][C:7]([NH:9][C:10]1[C:14]([C:15]([O:17]C)=O)=[CH:13][S:12][CH:11]=1)=[O:8].Cl.[F:20][C:21]1[CH:34]=[CH:33][C:24]([C:25]([CH:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)=[O:26])=[CH:23][CH:22]=1.C(=O)(O)[O-].[Na+].[I-].[Na+].NC1C(C(OC)=O)=CSC=1.BrCCCCN=C=O>C(O)(C)C.C1(C)C=CC=CC=1>[F:20][C:21]1[CH:22]=[CH:23][C:24]([C:25]([CH:27]2[CH2:32][CH2:31][N:30]([CH2:2][CH2:3][CH2:4][CH2:5][N:6]3[C:15](=[O:17])[C:14]4=[CH:13][S:12][CH:11]=[C:10]4[NH:9][C:7]3=[O:8])[CH2:29][CH2:28]2)=[O:26])=[CH:33][CH:34]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 5238Sodium IodideHCID 516892Sodium BicarbonateHCID 2777610Methyl 4-aminothiophene-3-carboxylateHCID 3084438p-Fluorophenyl 4-piperidyl ketone hydrochlorideHCID 149715841-Bromo-4-isocyanatobutaneHCID 15697666N-(4-bromobutyl)-N'-(4-carbomethoxythien-3-yl)urea

生成物 1

HCID 14500406
3-[4-[4-(4-Fluorobenzoyl)piperidin-1-yl]-butyl]thieno[3,4-d]pyrimidine-2,4-dione

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3776Isopropanol溶媒

実験手順

The title compound was prepared by dissolving N-(4-bromobutyl)-N'-(4-carbomethoxythien-3-yl)urea (6.92g, 21 mmol) in isopropanol (100 ml) and then successively treating the solution with 4-(4-fluorobenzoyl)piperidine hydrochloride (10.16 g, 42 mmol), sodium bicarbonate (3.7 g, 44 mmol) and sodium iodide (1.90 g, 12 mmol) to form a mixture. The urea was prepared by reacting methyl 4-aminothiophene-3-carboxylate with 4-bromobutylisocyanate in toluene at room temperature for 12 hours to produce the urea as a tan solid, mp 85°-86° C. The mixture was then heated to reflux under a nitrogen atmosphere for 12 hours. The reaction mixture was reduced to half volume, diluted with water, and concentrated to remove the remainder of the alcohol solvent. The residue was extracted with methylene chloride and the combined organic extracts were dried with saturated brine and magnesium sulfate. After concentration of the extracts, the residue was purified on silica gel using methylene chloride/ethanol/ammonium hydroxide (96:3.5:0.5) as eluant. There was obtained 3.62 g (40.8% yield) of the title compound as a brown solid. This material was recrystallized from CH2Cl2 /ether, mp 190°-192° C.

後処理

  1. customThe title compound was prepared
  2. customto form a mixture
  3. customThe urea was prepared
  4. customat room temperature
  5. customfor 12 hours

出典と根拠

ORDレコード
ord-d3d6e94072044445b35b2d1da6b7dff0
出典データセット
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04939137

反応ノート

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