1-Chloro-N,N-2-trimethylpropenylamine → HCID 59407570, compound

HRID 1093491Notes

Reaction equation

HRID 1093491 reaction equation
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH2:12][O:13][CH2:14][CH2:15][Si:16]([CH3:19])([CH3:18])[CH3:17])[CH2:6]O.[Cl:22]C(N(C)C)=C(C)C>C(Cl)Cl>[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH2:12][O:13][CH2:14][CH2:15][Si:16]([CH3:19])([CH3:18])[CH3:17])[CH2:6][Cl:22]

Participants

4

Reactant 2

HCID 6407921-Chloro-N,N-2-trimethylpropenylamineHCID 59407819HCID 59407819, compound

Product 1

HCID 59407570HCID 59407570, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

Compound 93-4 (28.5 g) was dissolved in methylene chloride (450 ml), 1-chloro-N,N,2-trimethyl-1-propenylamine (12.9 ml) was added under ice-cooling, and the mixture was stirred under ice-cooling for 1 hr. The reaction mixture was diluted with methylene chloride (200 ml), washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1-90:10) to give the object product (14.5 g) as a colorless oil.

Workup

  1. temperaturecooling
  2. temperaturecooling for 1 hr
  3. washwashed with water and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1-90:10)

Sources & evidence

ORD record
ord-481c25ff487b42d39eec122a662b5cd0
Source dataset
uspto-grants-2012_03
Patent number
US08129361B2

Reaction notes

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