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Dichloromethane → HCID 13648724, 화합물

HRID 2352526
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HRID 2352526 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6344Dichloromethane2회HCID 14798Sodium HydroxideHCID 27572524-tert-Butylbenzyl mercaptanHCID 13852600HCID 13852600, 화합물

생성물 1

HCID 13648724HCID 13648724, 화합물수율 70%

시약·촉매·용매 2

HCID 66133
Benzyl triethylammonium chloride
촉매
HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-bb6e4d5d0b82462ea0c90b5bccaad472
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04877787

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