Dimethylamine → HCID 20540231, compound

HRID 1065266Notes

Reaction equation

HRID 1065266 reaction equation
[CH3:1][NH:2][CH3:3].C(=O)([O-])[O-].[Na+].[Na+].O.[CH3:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2([C:29](Cl)=[O:30])[CH2:28][CH2:27][C:22]3([O:26][CH2:25][CH2:24][O:23]3)[CH2:21][CH2:20]2)=[CH:15][CH:14]=1>CC1C=CC=CC=1>[CH3:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2([C:29]([N:2]([CH3:3])[CH3:1])=[O:30])[CH2:28][CH2:27][C:22]3([O:26][CH2:25][CH2:24][O:23]3)[CH2:21][CH2:20]2)=[CH:15][CH:14]=1

Participants

6

Reactant 4

HCID 674DimethylamineHCID 962WaterHCID 10340Sodium CarbonateHCID 20540243HCID 20540243, compound

Product 1

HCID 20540231HCID 20540231, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

To a stirred and cooled (<0° C.) mixture of 49.5 parts of N-methylmethanamine solution 40%, 93 parts of sodium carbonate and 1000 parts of water is added dropwise a solution of 124 parts of 8-(4-methoxyphenyl)-1,4-dioxaspiro[4,5]decane-8-carbonyl chloride in 675 parts of methylbenzene. Upon completion, stirring is continued overnight at room temperature. The layers are separated and the organic phase is washed with water, dried, filtered and evaporated, yielding 128 parts (100%) of 8-(4-methoxyphenyl)-N,N-dimethyl-1,4-dioxaspiro[4,5]decane-8-carboxamide as a residue.

Workup

  1. temperaturecooled
  2. stirringUpon completion, stirring
  3. customThe layers are separated
  4. washthe organic phase is washed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated

Sources & evidence

ORD record
ord-57636b6782d74dd7b10a71b904a9c14c
Source dataset
uspto-grants-1982_05
Patent number
US04329353

Reaction notes

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