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Water → 1,2-Dimethyl-10-(3-chloropropyl)phenothiazine

HRID 48185
ノート
印刷プレビュー

反応式

HRID 48185 の反応式
[CH3:1][C:2]1[C:15]2[NH:14][C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[S:7][C:6]=2[CH:5]=[CH:4][C:3]=1[CH3:16].[H-].[Na+].[Cl:19][CH2:20][CH2:21][CH2:22]I.O>CN(C=O)C>[CH3:1][C:2]1[C:15]2[N:14]([CH2:22][CH2:21][CH2:20][Cl:19])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[S:7][C:6]=2[CH:5]=[CH:4][C:3]=1[CH3:16]
参加物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 962WaterHCID 24758Sodium hydrideHCID 813631-Chloro-3-iodopropaneHCID 227424451,2-Dimethylphenothiazine

生成物 1

HCID 227424361,2-Dimethyl-10-(3-chloropropyl)phenothiazine収率 57.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 5.0 g of 1,2-dimethylphenothiazine in N,N′-dimethylformamide was added 970 mg of sodium hydride under stirring at room temperature. After stirring at room temperature for 30 min, 4.0 g of 1-chloro-3-iodopropane was added dropwise followed by stirring at room temperature overnight. After adding water, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate. After evaporating the solvent under reduced pressure, the residue was purified by silica gel column chromatography to give 3.4 g of the title compound.

後処理

  1. stirringAfter stirring at room temperature for 30 min
  2. stirringby stirring at room temperature overnight
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customAfter evaporating the solvent under reduced pressure
  7. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-983d13628ac74d859a09faafa7a4c6fa
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06703388B2

反応ノート

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