Water → HCID 14622959, 화합물

HRID 1164789노트

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HRID 1164789 반응식
[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8]([SH:13])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[CH3:14][C:15]1[CH:24]=[CH:23][CH:22]=[C:21]([CH3:25])[C:16]=1[O:17][CH2:18][CH2:19]Br.C(=O)([O-])[O-].[Na+].[Na+].O>CN(C)C=O>[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8]([S:13][CH2:19][CH2:18][O:17][C:16]2[C:21]([CH3:25])=[CH:22][CH:23]=[CH:24][C:15]=2[CH3:14])[CH:7]=[N:6]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 24522082-(2-Bromoethoxy)-1,3-dimethylbenzeneHCID 134692424-Chloro-2-(1,1-dimethylethyl)-5-mercapto-3(2H)-pyridazinone

생성물 1

HCID 14622959HCID 14622959, 화합물수율 95%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 30 mm of N,N-dimethylformamide was dissolved 2.2 g of 2-t-butyl-4-chloro-5-mercapto-3(2H)-pyridazinone and 2.3 g of 2-(2',6'-dimethylphenoxy)ethyl bromide, and thereto were added 1.1 g of anhydrous sodium carbonate. The resulting solution was stirred at room temperature for fifteen hours. This solution was poured into water and extracted with diethyl ether. The organic layer was dried over anhydrous sodium sulfate and freed of solvent under reduced pressure to give crystals. The crystals thus obtained were washed with n-hexane to give 3.5 g of the intended compound. m.p. 104.3°~105.2° C.

후처리

  1. extractionextracted with diethyl ether
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customto give crystals
  4. customThe crystals thus obtained
  5. washwere washed with n-hexane

출처 및 근거

ORD 기록
ord-22fd11b800904dad95de3e2b6e1d2aba
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04906627

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