Cyanuric chloride → 6-chloro-2-N,4-N-bis[3-(diethylamino)propyl]-1,3,5-triazine-2,4-diamine

HRID 1164560

反応式

HRID 1164560 の反応式
[N:1]1[C:8](Cl)=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].[CH2:10]([N:12]([CH2:17][CH3:18])[CH2:13][CH2:14][CH2:15][NH2:16])[CH3:11].C(=O)([O-])[O-].[K+].[K+]>O>[Cl:3][C:2]1[N:1]=[C:8]([NH:16][CH2:15][CH2:14][CH2:13][N:12]([CH2:17][CH3:18])[CH2:10][CH3:11])[N:7]=[C:5]([NH:16][CH2:15][CH2:14][CH2:13][N:12]([CH2:17][CH3:18])[CH2:10][CH3:11])[N:4]=1

参加物

5

反応物 3

HCID 7954Cyanuric chlorideHCID 11430Potassium CarbonateHCID 61011N,N-Diethyl-1,3-propanediamine

生成物 1

HCID 1159956-chloro-2-N,4-N-bis[3-(diethylamino)propyl]-1,3,5-triazine-2,4-diamine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Following the procedure described in Japanese Patent Publication No. 39272/74, 50.0 ml of water was cooled to 3° C. and slowly 18.4 g (0.1 mole) of cyanuric chloride was added while maintaining 3°-5° C. by means of an external ice-water bath. Slowly 26.0 g (0.2 mole) of 3-(diethylamino)propylamine was added while maintaining 3°-12° C. by means of an ice-water bath. The resulting solution was stirred at ambient temperature for approximately eight hours and allowed to stand overnight. Slowly a 10 percent aqueous potassium carbonate solution was added to the reaction solution until it was slightly alkaline. The solid which precipitated was collected by filtration. The water wet filter cake was resuspended in water and dissolved by the addition of hydrochloric acid. Slowly 10 percent aqueous potassium carbonate was added until the mixture was slightly alkaline. The resulting solid was collected by filtration, washed with water and dried in vacuo to obtain 2-chloro-4,6-bis[3-(diethylamino)propyl]amino-1,3,5-triazine, a water-insoluble, white colored solid which melted at 119° C.

後処理

  1. temperaturewhile maintaining 3°-5° C. by means of an external ice-water bath
  2. temperaturewhile maintaining 3°-12° C. by means of an ice-water bath
  3. waitto stand overnight
  4. customThe solid which precipitated
  5. filtrationwas collected by filtration
  6. dissolutiondissolved by the addition of hydrochloric acid
  7. additionSlowly 10 percent aqueous potassium carbonate was added until the mixture
  8. filtrationThe resulting solid was collected by filtration
  9. washwashed with water
  10. customdried in vacuo

出典と根拠

ORDレコード
ord-7c9b41e1354f4332b6a57a20d4b59deb
出典データセット
uspto-grants-1983_01
特許番号
US04370443

関連ノート

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