2-Ethyl-2-nitro-1,3-propanediol → Nepd hmda

HRID 2064909

반응식

HRID 2064909 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][NH2:8].[N+:9]([C:12]([CH2:17][CH3:18])([CH2:15][OH:16])[CH2:13][OH:14])([O-:11])=[O:10].C(C([N+]([O-])=O)(CC)CO)C>>[CH3:18][CH2:17][C:12]([N+:9]([O-:11])=[O:10])([CH2:15][OH:16])[CH2:13][OH:14].[CH2:5]([CH2:6][CH2:7][NH2:8])[CH2:4][CH2:3][CH2:2][NH2:1]

참가 물질

4

반응물 3

HCID 116962-Ethyl-2-nitro-1,3-propanediolHCID 16402HexamethylenediamineHCID 208295982-Ethyl-2-nitrobutanol

생성물 1

HCID 131729996Nepd hmda

실험 절차

To a 1 neck round bottom flask equipped with stir bar and dropping funnel capped with a nitrogen outlet was added hexamethylenediamine (HMDA) (20 g, 0.17 mol). A 55% aqueous solution of the mixture of 2-nitro-2-ethyl-1,3-propanediol and 2-ethyl-2-nitrobutanol (189 g, 0.69 mol) was added drop wise to the flask over a period of 1 h with continuous stirring. After complete addition, the dropping funnel was replaced by a condenser and the reaction mixture refluxed for 6 h and stirred at room temperature overnight. After completion of the reaction, the content of the flask was filtered through suction filtration and the deep red high viscous material was collected and dried under vacuum for 8 h. The molecule was too bulky to be detected in GC/MS. The sample was passed through the HPLC Column (90/10 water/acetonitrile) and it showed the formation of three different products. The HPLC retention times recorded were 1.27, 1.66 and 1.91 minutes, with the most polar compound i.e., retention time 1.27 min was formed in greatest amount.

후처리

  1. customTo a 1 neck round bottom flask equipped
  2. customcapped with a nitrogen outlet
  3. additionwas added drop wise to the flask over a period of 1 h with continuous stirring
  4. additionAfter complete addition
  5. customthe dropping funnel was replaced by a condenser
  6. temperaturethe reaction mixture refluxed for 6 h
  7. stirringstirred at room temperature overnight
  8. customAfter completion of the reaction
  9. filtrationthe content of the flask was filtered through suction filtration
  10. customthe deep red high viscous material was collected
  11. customdried under vacuum for 8 h
  12. custom1.27, 1.66 and 1.91 minutes
  13. customwith the most polar compound i.e., retention time 1.27 min was formed in greatest amount

출처 및 근거

ORD 기록
ord-0a133fc503904549bd0394db086bb67b
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288464B2

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