Iodoethane → L 11204

HRID 1733131ノート

反応式

HRID 1733131 の反応式
[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]

参加物

5

反応物 3

HCID 6340Iodoethane2 回HCID 134401m-(5,6-Dihydro-s-triazolo(5,1-a)isoquinolin-2-yl)phenolHCID 2723922Sodium ethoxide

生成物 1

HCID 119282L 11204

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-002d50ccb2624136b497e578878b5b7b
出典データセット
uspto-grants-1980_12
特許番号
USRE030456

反応ノート

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