Ethanol → HCID 54461106、化合物

HRID 616722ノート

反応式

HRID 616722 の反応式
[C:1]1([C:7]2[C:19]([C:20]([OH:22])=[O:21])=[C:10]3[C:11]4[C:16]([CH2:17][CH2:18][N:9]3[N:8]=2)=[CH:15][CH:14]=[CH:13][CH:12]=4)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O=S(Cl)Cl.C(=O)(O)[O-].[Na+].[CH2:32](O)[CH3:33]>>[CH2:32]([O:21][C:20]([C:19]1[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:8][N:9]2[CH2:18][CH2:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]=12)=[O:22])[CH3:33]

参加物

5

反応物 4

HCID 702EthanolHCID 24386Thionyl Chloride2 回HCID 516892Sodium BicarbonateHCID 12948308HCID 12948308、化合物

生成物 1

HCID 54461106HCID 54461106、化合物

実験手順

2-Phenyl-5,6-dihydro-pyrazolo[5,1-a]isoquinoline-1-carboxylic acid (7.48 g.) is stirred at 90° C. for three hours with 3.77 ml. of SOCl2. The thionyl chloride excess is eliminated in vacuo and the residual acid chloride is dissolved in 80 ml. of ethanol at 40°-50° C. After 15 minutes, the reaction mixture is neutralized by addition of aqueous sodium bicarbonate and the solvent is eliminated by distillation. The residue is extracted with ethyl ether and, after evaporation of the organic solution, is crystallized from isopropyl ether. Yield of title compound 2.47 g.; m.p. 84°-5° C.

後処理

  1. customat 40°-50° C
  2. distillationthe solvent is eliminated by distillation
  3. extractionThe residue is extracted with ethyl ether
  4. customafter evaporation of the organic solution
  5. customis crystallized from isopropyl ether

出典と根拠

ORDレコード
ord-320aeeb2af37423dbca0ebc841aa7c77
出典データセット
uspto-grants-1978_02
特許番号
US04075342

反応ノート

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