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Dichloromethane → HCID 13648724、化合物

HRID 2352526
ノート
印刷プレビュー

反応式

HRID 2352526 の反応式
[OH-].[Na+].ClCCl.[C:6]([N:10]1[C:15](=[O:16])[C:14]([Br:17])=[C:13](Br)[CH:12]=[N:11]1)([CH3:9])([CH3:8])[CH3:7].[C:19]([C:23]1[CH:30]=[CH:29][C:26]([CH2:27][SH:28])=[CH:25][CH:24]=1)([CH3:22])([CH3:21])[CH3:20]>O.[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C>[C:6]([N:10]1[C:15](=[O:16])[C:14]([Br:17])=[C:13]([S:28][CH2:27][C:26]2[CH:29]=[CH:30][C:23]([C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:24][CH:25]=2)[CH:12]=[N:11]1)([CH3:9])([CH3:8])[CH3:7]
参加物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 6344Dichloromethane2 回HCID 14798Sodium HydroxideHCID 27572524-tert-Butylbenzyl mercaptanHCID 13852600HCID 13852600、化合物

生成物 1

HCID 13648724HCID 13648724、化合物収率 70%

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride
触媒
HCID 962Water溶媒

実験手順

Sodium hydroxide 0.22 g was dissolved in 5 ml of water, and thereto were added 10 ml of dichloromethane, 1.55 g of 2-tert.-butyl-4,5-dibromo-3(2H)-pyridazinone and 0.05 g of triethylbenzylammonium chloride. The resulting solution was incorporated with 0.83 g of 4-tert.-butyl-benzyl mercaptan at room temperature and then stirred for 10 hours. After completion of the reaction, about 50 ml of CH2Cl2 was added to the solution and the organic layer was separated therefrom, washed with 5% aqueous solution of sodium hydroxide and then with water, and dried over anhydrous sodium sulfate. Solvent was distilled away therefrom under reduced pressure and the resulting solid residue was recrystallized from a benzene/n-hexane mixed solvent to obtain 1.32 g of the intended compound (yield: 65%).

後処理

  1. additionwas added to the solution
  2. customthe organic layer was separated
  3. washwashed with 5% aqueous solution of sodium hydroxide
  4. dry with materialwith water, and dried over anhydrous sodium sulfate
  5. distillationSolvent was distilled away
  6. customunder reduced pressure and the resulting solid residue was recrystallized from a benzene/n-hexane mixed solvent

出典と根拠

ORDレコード
ord-bb6e4d5d0b82462ea0c90b5bccaad472
出典データセット
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04877787

反応ノート

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