Sodium Hydroxide → HCID 13590769, compound

HRID 1249347Notes

Reaction equation

HRID 1249347 reaction equation
[OH-].[Na+].[CH2:3]1[CH:12]2[CH:7]([O:8][C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[O:11]2)[CH:6]([OH:17])[CH2:5][CH2:4]1.Cl.Cl[CH2:20][CH2:21][N:22]1[CH2:27][CH2:26][O:25][CH2:24][CH2:23]1>>[O:25]1[CH2:26][CH2:27][N:22]([CH2:21][CH2:20][O:17][CH:6]2[CH:7]3[O:8][C:9]4[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=4[O:11][CH:12]3[CH2:3][CH2:4][CH2:5]2)[CH2:23][CH2:24]1

Participants

4

Reactant 3

HCID 14798Sodium HydroxideHCID 77210Morpholine, 4-(2-chloroethyl)-, hydrochloride (1:1)HCID 13590767HCID 13590767, compound

Product 1

HCID 13590769HCID 13590769, compound

Procedure

In a 10-liter reactor there were introduced 6 kg of 50% caustic soda solution, 1,150 g (5.576 moles) of the alcohol of Example 1, 986 g (5.3 moles) of 4-(2-chloroethyl)morpholine hydrochloride and 0.5 g of crown ether 18-crown-6 (1,4,7,10,13,16-hexaoxacycloocta-decane), and the mixture was then brought to 120° C. for 5 hours with stirring. After being cooled, the mixture was extracted with ether and the extract was washed with water dried over Na2SO4 and filtered, the solvent was evaporated and the product distilled under vacuum. There were thus obtained 1,330 g of the title-compound of boiling point 180° C. at a pressure of 65 Pa, having the elementary analysis:

Workup

  1. temperatureAfter being cooled
  2. extractionthe mixture was extracted with ether
  3. washthe extract was washed with water
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent was evaporated
  7. distillationthe product distilled under vacuum

Sources & evidence

ORD record
ord-1fa55ebd3fae454dbe8aacc55943c5dc
Source dataset
uspto-grants-1986_12
Patent number
US04631277

Reaction notes

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