Carbon Dioxide → HCID 86759733, compound

HRID 2182635Notes

Reaction equation

HRID 2182635 reaction equation
[CH:1]1[CH:2]=[CH:3][C:4]2[N:9]([OH:10])[N:8]=[N:7][C:5]=2[CH:6]=1.O.C(N)C.C(=O)=O>CC(C)=O>[CH2:5]([NH2:7])[CH3:4].[CH:1]1[CH:2]=[CH:3][C:4]2[N:9]([OH:10])[N:8]=[N:7][C:5]=2[CH:6]=1

Participants

6

Reactant 4

HCID 280Carbon DioxideHCID 962WaterHCID 6341EthylamineHCID 757711-Hydroxybenzotriazole

Product 1

HCID 86759733HCID 86759733, compoundYield 217.1%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

11.58 g (77.2 mmol) of HOBt are weighed out in a 2-L flask. 1 L of water is added and the flask submerged in an ultrasound bath until dispersion is complete. 6.18 mL (103.1 mmol) of ethylamine are added, maintaining the ultrasonification. The dispersion is seen to dissolve completely. The transparent solution is allowed to stand for 5 minutes at room temperature. It is then frozen in a bath of dry ice and acetone. It is lyophilised. Once well lyophilised the product is withdrawn from the flask and collected in a beaker. The solid is left to dry under vacuum in the presence of KOH for at least 24 hours, to give 15.1 g of the salt of ethylamine/HOBt.

Workup

  1. customthe flask submerged in an ultrasound bath until dispersion
  2. temperaturemaintaining the ultrasonification
  3. dissolutionto dissolve completely
  4. customis withdrawn from the flask
  5. customcollected in a beaker
  6. waitThe solid is left
  7. dry with materialto dry under vacuum in the presence of KOH for at least 24 hours

Sources & evidence

ORD record
ord-6f5d0b8d3cb541a49f0afb0caffc967e
Source dataset
uspto-grants-2005_05
Patent number
US06897289B1

Reaction notes

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