1-Hexanol → N-cyclohexyl-p-phenylenedamine

HRID 3982

反応式

HRID 3982 の反応式
[CH:1]1([NH:7][C:8]2[CH:13]=[CH:12][C:11]([N:14]=O)=[CH:10][CH:9]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[OH-].[Na+].C(O)CCCCC>>[CH:1]1([NH:7][C:8]2[CH:9]=[CH:10][C:11]([NH2:14])=[CH:12][CH:13]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

4

反応物 3

HCID 81031-HexanolHCID 14798Sodium HydroxideHCID 20065262N-cyclohexyl-4-nitrosoaniline

生成物 1

HCID 2771376N-cyclohexyl-p-phenylenedamine

反応条件

温度
95 °C

実験手順

51.0 g (0.25 mole) N-cyclohexyl-4-nitrosoaniline, 20.0 g (50%) NaOH and 135 g n-hexanol were charged to a 0.5 liter three-necked round bottom flask equipped with stirrer, condenser and thermometer, and heated while stirring to 95° C. until the development of an exotherm was observed. Heating was discontinued, the reaction temperature continued to rise to 115° C. and then dropped, within 10 minutes, to 100° C. With the application of heat, a temperature of 90°-95° C. was maintained for 30 minutes. The reaction mixture contained no unreacted nitroso compound. The yield of the product was 64 wt. %; m.p. 59°-61° C.

後処理

  1. customequipped with stirrer, condenser
  2. temperaturethermometer, and heated
  3. temperatureHeating
  4. customto rise to 115° C.
  5. additiondropped, within 10 minutes, to 100° C
  6. temperatureWith the application of heat
  7. temperaturea temperature of 90°-95° C. was maintained for 30 minutes

出典と根拠

ORDレコード
ord-37aa6ea9a1e04e1a9edfeac185572691
出典データセット
uspto-grants-1988_02
特許番号
US04723040

関連ノート

読み込み中…