Ethanol → HCID 54461106, 화합물

HRID 616722노트

반응식

HRID 616722 반응식
[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]

참가 물질

5

반응물 4

HCID 702EthanolHCID 24386Thionyl Chloride2회HCID 516892Sodium BicarbonateHCID 12948308HCID 12948308, 화합물

생성물 1

HCID 54461106HCID 54461106, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-320aeeb2af37423dbca0ebc841aa7c77
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04075342

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