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Sodium Iodide → HCID 42637597、化合物

HRID 1816179
ノート
印刷プレビュー

反応式

HRID 1816179 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=3)[S:11][CH:12]=2)=[CH:4][CH:3]=1.Br[CH2:25][C:26]1[CH:35]=[CH:34][C:29]([C:30]([O:32][CH3:33])=[O:31])=[CH:28][CH:27]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>C(#N)C>[CH3:33][O:32][C:30](=[O:31])[C:29]1[CH:34]=[CH:35][C:26]([CH2:25][N:13]([C:10]2[S:11][CH:12]=[C:8]([C:5]3[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=3)[N:9]=2)[C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:21])([F:23])[F:22])=[CH:16][CH:15]=2)=[CH:27][CH:28]=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

6

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 256687Methyl 4-(bromomethyl)benzoateHCID 22496401HCID 22496401、化合物

生成物 1

HCID 42637597HCID 42637597、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

[4-(4-Chlorophenyl)thiazol-2-yl]-(4-trifluoromethylphenyl)amine (0.335 mg; 0.95 mmol) was dissolved in acetonitril (4 ml) and methyl 4-(bromomethyl)benzoate (238 mg; 1.04 mmol), potassium carbonate (195 mg; 1.41 mmol) and sodium iodide (212 mg; 1.41 mmol) were added. The reaction mixture was heated to 60° C. for 3 days, then filtered while still hot. The solvent was removed by rotary evaporation, then the residue was dissolved in ethyl acetate (50 ml) and washed with water (50 ml) and brine (50 ml). The organic phase was dried with sodium sulphate, and taken to dryness by rotary evaporation. The residue was striped once with acetonitril to give pure 4-{[[4-(4-chlorophenyl)thiazol-2-yl]-(4-trifluoromethylphenyl)amino]methyl}benzoic acid methyl ester as an oil. Yield; 454 mg (96%).

後処理

  1. filtrationfiltered while still hot
  2. customThe solvent was removed by rotary evaporation
  3. dissolutionthe residue was dissolved in ethyl acetate (50 ml)
  4. washwashed with water (50 ml) and brine (50 ml)
  5. dry with materialThe organic phase was dried with sodium sulphate
  6. customtaken to dryness by rotary evaporation

出典と根拠

ORDレコード
ord-fb2ab84615dd4d65a33402d3a4e3d646
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06881746B2

反応ノート

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