3-Amino-1,2-propanediol → HCID 19778858、化合物

HRID 2081902ノート

反応式

HRID 2081902 の反応式
[N+:1]([C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([N+:11]([O-:13])=[O:12])[C:5]=1OC)([O-:3])=[O:2].[NH2:16][CH2:17][CH:18]([OH:21])[CH2:19][OH:20]>O>[N+:1]([C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([N+:11]([O-:13])=[O:12])[C:5]=1[NH:16][CH2:17][CH:18]([OH:21])[CH2:19][OH:20])([O-:3])=[O:2]

参加物

4

反応物 2

HCID 735613-Amino-1,2-propanediolHCID 2596494-Methoxy-3,5-dinitrotoluene

生成物 1

HCID 19778858HCID 19778858、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

0.05 mol (10.6 g) of 2,6-dinitro-4-methylanisole is dissolved in 50 ml of absolute alcohol. 0.1 mol (9.1 g) of 1-aminopropane-2,3-diol is added gradually to this solution, whilst stirring. The solution is heated under reflux for 3 hours 30 minutes. The alcohol is driven off in vacuo and 40 ml of iced water are added to the residual red oil. The expected product crystallises. It is filtered off and washed with water. After recrystallisation from an aqueous-alcoholic mixture and drying in vacuo, it melts at 118° C.

後処理

  1. temperatureThe solution is heated
  2. temperatureunder reflux for 3 hours 30 minutes
  3. additionare added to the residual red oil
  4. customThe expected product crystallises
  5. filtrationIt is filtered off
  6. washwashed with water
  7. customAfter recrystallisation from an aqueous-alcoholic mixture
  8. customdrying in vacuo, it melts at 118° C.

出典と根拠

ORDレコード
ord-434fa734567a434581b53d7c61d70a42
出典データセット
uspto-grants-1993_02
特許番号
US05186717

反応ノート

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