Ammonia → Hexamethylenediamine

HRID 615271

反応式

HRID 615271 の反応式
[CH2:1]([CH2:6][CH2:7][NH2:8])[CH2:2][CH2:3][CH2:4][NH2:5].[C:9](=[O:20])([O:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])N.N>>[CH2:12]([O:11][C:9]([NH:5][CH2:4][CH2:3][CH2:2][CH2:1][CH2:6][CH2:7][NH:8][C:9]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:20])=[O:20])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].[CH2:1]([CH2:6][CH2:7][NH2:8])[CH2:2][CH2:3][CH2:4][NH2:5]

参加物

5

反応物 3

HCID 222AmmoniaHCID 16240Carbamic acid, octyl esterHCID 16402Hexamethylenediamine

生成物 2

HCID 16402HexamethylenediamineHCID 147932871,6-Bis(octoxycarbonylamino)hexane

反応条件

温度
110 °C

実験手順

Agitated in a reaction vessel are 116 parts of 1,6-hexamethylenediamine with 380 parts of O-octyl carbamate and 130 parts of n-octanol-(1) at a reflux temperature of 185° C.-205° C. for 2 hours while the ammonia is removed by distillation. At this point, an additional 500 parts of n-octanol-(1) are allowed to flow into the reaction mixture and the reaction is continued at reflux temperature for 7 hours. The reaction mixture, cooled to 110° C., is filtered, and the reaction product is allowed to crystallize by cooling. By filtration, washing with n-octanol-(1) and drying, 388 parts of 1,6-bis(octoxycarbonylamino)hexane are obtained corresponding with 90.6 percent theory relative to 1,6-hexamethylenediamine. The melting point is 107° C.-109° C.

後処理

  1. customat a reflux temperature of 185° C.-205° C.
  2. customfor 2 hours
  3. customis removed by distillation
  4. temperatureat reflux temperature for 7 hours
  5. filtrationis filtered
  6. customto crystallize
  7. temperatureby cooling
  8. filtrationBy filtration
  9. washwashing with n-octanol-(1)
  10. customdrying

出典と根拠

ORDレコード
ord-5332610378834358be6b062ba15740f7
出典データセット
uspto-grants-1985_02
特許番号
US04497963

関連ノート

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