3-Amino-1,2-propanediol → HCID 19778858, 화합물

HRID 2081902노트

반응식

HRID 2081902 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 19778858HCID 19778858, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-434fa734567a434581b53d7c61d70a42
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05186717

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