Toluene → Cyclohexylmelamine

HRID 365707

反応式

HRID 365707 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4](Cl)[N:3]=1.[CH:10]1([NH2:16])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1.[OH-].[Na+].C1(C)C=CC=CC=1>O>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([NH:16][CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[N:3]=1

参加物

6

反応物 4

HCID 1140TolueneHCID 7965CyclohexylamineHCID 14798Sodium HydroxideHCID 188311,3,5-Triazine-2,4-diamine, 6-chloro-

生成物 1

HCID 134592Cyclohexylmelamine収率 86%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixed solution of 14.5 g (0.1 mol) of 2,4-diamino-6-chloro-1,3,5-triazine prepared in Reference Example 1, 140 mL of water, and 29.2 g (0.3 mol) of cyclohexylamine was warmed with stirring and allowed to react at a reflux temperature for 1 hour. Further, an aqueous solution of 12 g of sodium hydroxide in 40 mL of water was dropwise added thereto over 1 hour and the mixture was aged for 1 hour. To the reaction mixture thus obtained was added 200 mL of toluene, and the resulting mixture was cooled down to room temperature. The crystals obtained were collected by filtration, washed with 100 mL of toluene and then with 100 mL of water, followed by drying under reduced pressure to obtain 17.9 g (yield 86%) of the titled compound. Melting point: 151° C.

後処理

  1. temperaturewas warmed
  2. customto react at a reflux temperature for 1 hour
  3. waitthe mixture was aged for 1 hour
  4. customTo the reaction mixture thus obtained
  5. customThe crystals obtained
  6. filtrationwere collected by filtration
  7. washwashed with 100 mL of toluene
  8. customby drying under reduced pressure

出典と根拠

ORDレコード
ord-62bb90f061f14a2cbe2c6cd7ba58f228
出典データセット
uspto-grants-2000_10
特許番号
US06127538

関連ノート

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