2,4-Dichloro-6-methoxyphenol → HCID 21495080、化合物

HRID 1731118ノート

反応式

HRID 1731118 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([O:9][CH3:10])[C:3]=1[OH:11].[CH3:12]C[O-].[Na+].[Na].ClC[CH2:19][CH2:20][N:21]1[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1>C(O)C>[O:24]1[CH2:25][CH2:26][N:21]([CH2:20][CH2:19][CH2:10][O:9][C:4]2[CH:5]=[C:6]([Cl:8])[CH:7]=[C:2]([Cl:1])[C:3]=2[O:11][CH3:12])[CH2:22][CH2:23]1

参加物

6

反応物 4

HCID 280512,4-Dichloro-6-methoxyphenolHCID 958344-(3-Chloropropyl)morpholineHCID 2723922Sodium ethoxideHCID 5360545Sodium

生成物 1

HCID 21495080HCID 21495080、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

54 g of 3,5-dichloroguaiacol (0.28 mole) is added to sodium ethylate produced by reacting 6.44 g of sodium on 84 ml of ethyl alcohol. 51 g (0.28 mole + 10% excess) of 1-chloro-3-morpholinopropane is added to the resulting solution. The mixture is heated under reflux for 8 hours. Precipitation of sodium chloride is observed. Cooling is effected and then the mixture is dissolved in 300 ml of water and 30 ml of concentrated hydrochloric acid. The resulting solution is filtered, then ammonia is added to precipitate the base which is extracted with ether. The ether is eliminated and the residue is distilled under vacuum.

後処理

  1. customproduced
  2. temperatureThe mixture is heated
  3. temperatureunder reflux for 8 hours
  4. customPrecipitation of sodium chloride
  5. temperatureCooling
  6. dissolutionthe mixture is dissolved in 300 ml of water
  7. filtrationThe resulting solution is filtered
  8. additionammonia is added
  9. customto precipitate the base which
  10. extractionis extracted with ether
  11. distillationthe residue is distilled under vacuum

出典と根拠

ORDレコード
ord-1ae9b7a710e4427ba435779ae436bfde
出典データセット
uspto-grants-1976_11
特許番号
US03995037

反応ノート

読み込み中…