Sodium Hydroxide → HCID 178457593, 화합물

HRID 1973117

반응식

HRID 1973117 반응식
[ClH:1].[CH3:2][CH:3]([NH2:14])[C:4]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][CH:5]=1.[CH:15]([NH:18][C:19]([NH:21][C:22]#[N:23])=[NH:20])([CH3:17])[CH3:16].[OH-].[Na+]>O>[ClH:1].[ClH:1].[CH3:2][CH:3]([NH:14][C:22]([NH:21][C:19]([NH:18][CH:15]([CH3:17])[CH3:16])=[NH:20])=[NH:23])[C:4]1[CH:5]=[CH:6][C:7]([C:10]([F:11])([F:12])[F:13])=[CH:8][CH:9]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 214929691-(4-(Trifluoromethyl)phenyl)ethanamine hydrochlorideHCID 178457589HCID 178457589, 화합물

생성물 1

HCID 178457593HCID 178457593, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A stirred mixture of 15.5 g (0.0687 mole) of α-methyl-p-trifluoromethylbenzylamine hydrochloride and 9.55 g (0.0756 mole) of 1-i-propyl-3-cyanoguanidine is immersed in a 190° C oil bath for ten minutes. The melt is cooled to room temperature, dissolved in 100 ml of water, made alkaline with 40% sodium hydroxide solution and extracted twice with 200 ml of ether. The combined ether extracts are dried over potassium carbonate, filtered, and the ether solution made strongly acidic with a saturated ethereal hydrochloric acid ether solution. The precipitate is collected on a filter, washed twice with 50 ml of anhydrous ether, and dried at 40°C/125 mm. for 5 hours. The dihydrochloride is dissolved in 50 ml of water, made strongly alkaline with 40% sodium hydroxide solution, and extracted twice with 100 ml of ether. The combined ether extracts are dried over potassium carbonate, filtered, and the ether solution made strongly acidic with a saturated ethereal hydrochloric acid solution. The precipitate is collected on a filter, washed twice with 50 ml of anhydrous ether, and dried at 40° C/125 mm. to obtain 1-(α-methyl-p-trifluoromethylbenzyl)-5-i-propylbiguanide dihydrochloride.

후처리

  1. customis immersed in a 190° C
  2. customfor ten minutes
  3. extractionextracted twice with 200 ml of ether
  4. dry with materialThe combined ether extracts are dried over potassium carbonate
  5. filtrationfiltered
  6. customThe precipitate is collected on a filter
  7. washwashed twice with 50 ml of anhydrous ether
  8. customdried at 40°C/125 mm
  9. dissolutionThe dihydrochloride is dissolved in 50 ml of water
  10. extractionextracted twice with 100 ml of ether
  11. dry with materialThe combined ether extracts are dried over potassium carbonate
  12. filtrationfiltered
  13. customThe precipitate is collected on a filter
  14. washwashed twice with 50 ml of anhydrous ether
  15. customdried at 40° C/125 mm

출처 및 근거

ORD 기록
ord-318b7b81f1f249558e64ad4b6aac0594
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996232

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