Sodium Hydroxide → HCID 178457593、化合物

HRID 1973117ノート

反応式

HRID 1973117 の反応式
[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

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 214929691-(4-(Trifluoromethyl)phenyl)ethanamine hydrochlorideHCID 178457589HCID 178457589、化合物

生成物 1

HCID 178457593HCID 178457593、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-318b7b81f1f249558e64ad4b6aac0594
出典データセット
uspto-grants-1976_12
特許番号
US03996232

反応ノート

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