2-Chloroethanol → HCID 12688574、化合物

HRID 1732648ノート

反応式

HRID 1732648 の反応式
[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

参加物

6

反応物 4

HCID 342-ChloroethanolHCID 6228DimethylformamideHCID 14798Sodium HydroxideHCID 3599665HCID 3599665、化合物

生成物 1

HCID 12688574HCID 12688574、化合物収率 25%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6cd112bbb4c24225bfd38133c2bb0262
出典データセット
uspto-grants-1980_12
特許番号
US04238490

反応ノート

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