Sodium Hydroxide → 1-(p-Trifluoromethylbenzyl)-5-i-propylbiguanide dihydrochloride

HRID 1973116노트

반응식

HRID 1973116 반응식
[ClH:1].[F:2][C:3]([F:13])([F:12])[C:4]1[CH:11]=[CH:10][C:7]([CH2:8][NH2:9])=[CH:6][CH:5]=1.[CH:14]([NH:17][C:18]([NH:20][C:21]#[N:22])=[NH:19])([CH3:16])[CH3:15].[OH-].[Na+]>O>[ClH:1].[ClH:1].[F:2][C:3]([F:12])([F:13])[C:4]1[CH:11]=[CH:10][C:7]([CH2:8][NH:9][C:21]([NH:20][C:18]([NH:17][CH:14]([CH3:16])[CH3:15])=[NH:19])=[NH:22])=[CH:6][CH:5]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 160903514-(Trifluoromethyl)benzylamine HydrochlorideHCID 178457589HCID 178457589, 화합물

생성물 1

HCID 1784575911-(p-Trifluoromethylbenzyl)-5-i-propylbiguanide dihydrochloride

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A stirred mixture of 6.9 g (0.035 mole) of p-trifluoromethylbenzylamine hydrochloride and 4.3 (0.035 mole) of 1-i-propyl-3-cyanoguanidine is immersed in a 180° C oil bath for 1 hour. The melt is cooled and dissolved in 35 ml of hot water. The solution is cooled in an ice bath, made alkaline with 40% sodium hydroxide solution, and extracted with 150 ml of ether. The ether layer is dried over potassium carbonate, filtered and the ether solution made strongly acidic with a saturated ethereal hydrochloric acid solution. The precipitate is washed twice with 25 ml of anhydrous ether and recrystallized from a mixture of ethanol and heptane (3:5) to obtain 1-(p-trifluoromethylbenzyl)-5-i-propylbiguanide dihydrochloride.

후처리

  1. customis immersed in a 180° C
  2. customfor 1 hour
  3. temperatureThe melt is cooled
  4. temperatureThe solution is cooled in an ice bath
  5. extractionextracted with 150 ml of ether
  6. dry with materialThe ether layer is dried over potassium carbonate
  7. filtrationfiltered
  8. washThe precipitate is washed twice with 25 ml of anhydrous ether
  9. customrecrystallized from a mixture of ethanol and heptane (3:5)

출처 및 근거

ORD 기록
ord-6642f07e15244849b08bd6e1fa69b90e
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996232

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