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Potassium Iodide → N-(4-(1-(4-(4-fluorophenyl)piperazin-1-yl)-1-methylethyl)phenylmethyl)acetamide dihydrochloride monohydrate

HRID 1282124
ノート
印刷プレビュー

反応式

HRID 1282124 の反応式
[NH2:1][C:2]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH:12][C:13](=[O:15])[CH3:14])=[CH:7][CH:6]=1)([CH3:4])[CH3:3].[Cl:16][CH2:17][CH2:18][N:19]([CH2:27][CH2:28]Cl)[C:20]1[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CS(C)=O.O>[OH2:15].[ClH:16].[ClH:16].[F:26][C:23]1[CH:24]=[CH:25][C:20]([N:19]2[CH2:27][CH2:28][N:1]([C:2]([C:5]3[CH:10]=[CH:9][C:8]([CH2:11][NH:12][C:13](=[O:15])[CH3:14])=[CH:7][CH:6]=3)([CH3:3])[CH3:4])[CH2:17][CH2:18]2)=[CH:21][CH:22]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 30941Aniline, N,N-bis(2-chloroethyl)-p-fluoro-HCID 18423109N-(4-(1-amino-1-methylethyl)phenylmethyl)acetamide

生成物 1

HCID 18423145N-(4-(1-(4-(4-fluorophenyl)piperazin-1-yl)-1-methylethyl)phenylmethyl)acetamide dihydrochloride monohydrate収率 22.6%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To a solution of N-(4-(1-amino-1-methylethyl)phenylmethyl)-acetamide (1.55 g) and N,N-di(2-chloroethyl)-4-fluoroaniline (1.5 g) in dimethyl sulfoxide (30 ml) were added potassium carbonate (3.12 g) and potassium iodide (2.50 g) and the mixture was stirred at 80° C. for 24 hr. The reaction mixture was poured into water (300 ml) and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel chromatography (developing solvent; ethyl acetate:hexane=3:1) and treated with 1M hydrochloric acid-ether in ethanol to give the title compound (0.33 g) as white crystals.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated
  5. customthe obtained residue was purified by silica gel chromatography (developing solvent; ethyl acetate:hexane=3:1)
  6. additiontreated with 1M hydrochloric acid-ether in ethanol

出典と根拠

ORDレコード
ord-e5489caa0e9b47868fbcc60aa2f95bca
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06455528B1

反応ノート

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