Iodoethane → L 11204

HRID 616692노트

반응식

HRID 616692 반응식
[OH:1][C:2]1[CH:3]=[C:4]([C:8]2[N:20]=[C:11]3[C:12]4[C:17]([CH2:18][CH2:19][N:10]3[N:9]=2)=[CH:16][CH:15]=[CH:14][CH:13]=4)[CH:5]=[CH:6][CH:7]=1.[O-][CH2:22][CH3:23].[Na+].C(I)C>C(O)C>[CH2:22]([O:1][C:2]1[CH:3]=[C:4]([C:8]2[N:20]=[C:11]3[C:12]4[C:17]([CH2:18][CH2:19][N:10]3[N:9]=2)=[CH:16][CH:15]=[CH:14][CH:13]=4)[CH:5]=[CH:6][CH:7]=1)[CH3:23]

참가 물질

5

반응물 3

HCID 6340Iodoethane2회HCID 134401m-(5,6-Dihydro-s-triazolo(5,1-a)isoquinolin-2-yl)phenolHCID 2723922Sodium ethoxide

생성물 1

HCID 119282L 11204

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

2-(3-Hydroxyphenyl)-5,6-dihydro-s-triazolo-[5,1-a]isoquinoline (3.95 g.) is added to 60 ml. of ethanol containing one equivalent proportion of sodium ethoxide. To this mixture is added 1.57 ml. of ethyl iodide in 15 ml. of ethanol. After stirring for one hour at room temperature, a further 1.57 ml. of ethyl iodide is added and the mixture is refluxed for 18 hours. The solvent is distilled off and the residue is washed with water and extracted with dichloromethane. Evaporation of the solvent and crystallization of the residue from ethanol gives 3.87 g. of the title product; m.p. 102°-3° C.

후처리

  1. additionTo this mixture is added 1.57 ml
  2. temperaturethe mixture is refluxed for 18 hours
  3. distillationThe solvent is distilled off
  4. washthe residue is washed with water
  5. extractionextracted with dichloromethane
  6. customEvaporation of the solvent and crystallization of the residue from ethanol
  7. customgives 3.87 g

출처 및 근거

ORD 기록
ord-7eb89bf05afa4e17aa7912120d86889f
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04075341

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