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Hexylamine → N~2~-Hexyl-1,3,5-triazine-2,4,6-triamine

HRID 2163617
ノート
印刷プレビュー

反応式

HRID 2163617 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4](Cl)[N:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[CH2:16]([NH2:22])[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]>CN(C)C=O>[CH2:16]([NH:22][C:4]1[N:3]=[C:2]([NH2:1])[N:7]=[C:6]([NH2:8])[N:5]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8102HexylamineHCID 10340Sodium CarbonateHCID 188311,3,5-Triazine-2,4-diamine, 6-chloro-

生成物 1

HCID 19734692N~2~-Hexyl-1,3,5-triazine-2,4,6-triamine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A mixture of 72.8 g. (0.500 mole) of 2,4-diamino-6-chloro-s-triazine, 63.6 g. (0.600 mole) of anhydrous sodium carbonate, and 200 ml. of N,N-dimethylformamide (DMF) was heated over 43 minutes of 124° C. To this was added, over a period of 2.35 hours, a solution of 60.7 g. (0.600 mole) of n-hexylamine in 100 ml. of DMF; temperature was controlled at 122°-127° C. during the addition. The reaction mixture was heated for an additional 19 hours at 124°-125° C., then was filtered hot. The filter cake was washed with 100 ml of hot DMF, and the combined filtrate was cooled and added with stirring to about 5 liters of ice-water. The precipitate was recovered by filtration, reslurried with 3 liters of water, filtered again, washed thoroughly with deionized water, and dried to constant weight in a vacuum oven at 60° C. The yield of n-hexylmelamine, m.p. 115°-117.5° C., was 91.4 g. (87.0%).

後処理

  1. additionA mixture of 72.8 g
  2. additionTo this was added, over a period of 2.35 hours
  3. additiontemperature was controlled at 122°-127° C. during the addition
  4. temperatureThe reaction mixture was heated for an additional 19 hours at 124°-125° C.
  5. filtrationwas filtered hot
  6. washThe filter cake was washed with 100 ml of hot DMF
  7. temperaturethe combined filtrate was cooled
  8. additionadded
  9. filtrationThe precipitate was recovered by filtration
  10. filtrationfiltered again
  11. washwashed thoroughly with deionized water
  12. customdried to constant weight in a vacuum oven at 60° C

出典と根拠

ORDレコード
ord-6907d8de27b74d2596a39b1ffe679d7e
出典データセット
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04136092

反応ノート

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