Water → HCID 13563603, compound

HRID 638475Notes

Reaction equation

HRID 638475 reaction equation
[CH2:1]([C:3]1([NH2:9])[CH2:8][O:7][CH2:6][O:5][CH2:4]1)[CH3:2].[OH-].[Na+].O.[Cl:13][CH2:14][C:15](Cl)=[O:16]>C(Cl)Cl>[Cl:13][CH2:14][C:15]([NH:9][C:3]1([CH2:1][CH3:2])[CH2:8][O:7][CH2:6][O:5][CH2:4]1)=[O:16]

Participants

6

Reactant 4

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 14798Sodium HydroxideHCID 20249601HCID 20249601, compound

Product 1

HCID 13563603HCID 13563603, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Five and two-tenths g (0.04 mole) of 5-ethyl-5-amino-1,3-dioxane, 3.2 g (0.04 mole) of 50% sodium hydroxide, 10 ml of water, and 90 ml of methylene chloride were combined in a reaction flask. The mixture was cooled to below 35° C. Four and one-half g of chloroacetylchloride were added dropwise. The reaction mixture was stirred for one-half hour, washed with water and dried over magnesium sulfate. The solvent was vacuum stripped. Yield was 5.8 g of 5-chloroacetylamino-5-ethyl-1,3-dioxane. m.p.=89°-95° C. Structure was confirmed by NMR.

Workup

  1. temperatureThe mixture was cooled to below 35° C
  2. washwashed with water
  3. dry with materialdried over magnesium sulfate

Sources & evidence

ORD record
ord-13ace90e4f584e27be8b1ec695c89804
Source dataset
uspto-grants-1985_12
Patent number
US04561876

Reaction notes

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