2-Chloroethanol → HCID 12688574, 화합물

HRID 1732648노트

반응식

HRID 1732648 반응식
[C:1]1([C:7]2[C:8](=[O:25])[NH:9][N:10]=[C:11]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CN(C)C=O.[OH-].[Na+].Cl[CH2:34][CH2:35][OH:36]>O>[OH:36][CH2:35][CH2:34][N:9]1[C:8](=[O:25])[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[C:12]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:11]([C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)=[N:10]1

참가 물질

6

반응물 4

HCID 342-ChloroethanolHCID 6228DimethylformamideHCID 14798Sodium HydroxideHCID 3599665HCID 3599665, 화합물

생성물 1

HCID 12688574HCID 12688574, 화합물수율 25%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 4,5,6-triphenyl-2H-pyridazin-3-one (6.0 g) were added 50 ml of dimethylformamide and a solution of sodium hydroxide pellets (0.7 g) dissolved in 5 ml of water. The resultant slurry was stirred at room temperature, while adding dropwise, 1.5 g of 2-chloroethanol. The mixture was heated to 110° C. for 1 hour and then allowed to heat for 16 hours at 90° C., after which time, the dimethylformamide was removed by evacuation. The residue was redissolved in methanol from which the compound was triturated, filtered and washed with petroleum ether to obtain the title compound (25 percent yield), m.p. 189° C. (dec).

후처리

  1. additionwhile adding dropwise
  2. temperatureThe mixture was heated to 110° C. for 1 hour
  3. temperatureto heat for 16 hours at 90° C.
  4. customafter which time, the dimethylformamide was removed by evacuation
  5. dissolutionThe residue was redissolved in methanol from which the compound
  6. customwas triturated
  7. filtrationfiltered
  8. washwashed with petroleum ether

출처 및 근거

ORD 기록
ord-6cd112bbb4c24225bfd38133c2bb0262
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04238490

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