Ethylene Glycol → HCID 22767867, compound

HRID 2419277Notes

Reaction equation

HRID 2419277 reaction equation
C(OC([N:6]1[CH2:11][CH2:10][N:9]([CH:12]2[C:18]3[CH:19]=[C:20]([CH3:23])[CH:21]=[CH:22][C:17]=3[O:16][C:15]3[CH:24]=[CH:25][C:26]([CH3:28])=[CH:27][C:14]=3[CH2:13]2)[CH2:8][CH2:7]1)=O)C.[OH-].[K+].C(O)CO>O>[CH3:28][C:26]1[CH:25]=[CH:24][C:15]2[O:16][C:17]3[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][C:18]=3[CH:12]([N:9]3[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]3)[CH2:13][C:14]=2[CH:27]=1

Participants

5

Reactant 3

HCID 174Ethylene GlycolHCID 14797Potassium HydroxideHCID 54428684HCID 54428684, compound

Product 1

HCID 22767867HCID 22767867, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

22.0 G. of 4-[10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin-10-yl]-1-piperazinecarboxylic acid ethyl ester and 22 g. of potassium hydroxide are stirred in 320 ml. of ethyleneglycol and 1.5 ml. of water for 90 minutes at 160° C. After cooling, the mixture is diluted with 1.3 liters of water and extracted three times with ether. The ethereal extracts are washed twice with saturated sodium chloride solution, dried over sodium sulfate, evaporated in vacuo, and there is obtained crude 1-[10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin-10-yl]-piperazine as an oil.

Workup

  1. temperatureAfter cooling
  2. extractionextracted three times with ether
  3. washThe ethereal extracts are washed twice with saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo

Sources & evidence

ORD record
ord-c42072c9b2cc4380b0f61c8ca9615fd2
Source dataset
uspto-grants-1978_08
Patent number
US04105664

Reaction notes

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