Triethylamine → HCID 53858779, compound

HRID 1952819Notes

Reaction equation

HRID 1952819 reaction equation
C(N(CC)CC)C.[CH2:8]([N:26]=[C:27]=[O:28])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].[OH:29][CH2:30][C:31]1[CH:36]=[C:35]([O:37][CH3:38])[C:34]([O:39][CH3:40])=[CH:33][C:32]=1[CH2:41][C:42]([N:44]1[CH2:49][CH2:48][N:47]([CH3:50])[CH2:46][CH2:45]1)=[O:43]>ClCCl>[CH2:8]([NH:26][C:27](=[O:28])[O:29][CH2:30][C:31]1[CH:36]=[C:35]([O:37][CH3:38])[C:34]([O:39][CH3:40])=[CH:33][C:32]=1[CH2:41][C:42]([N:44]1[CH2:45][CH2:46][N:47]([CH3:50])[CH2:48][CH2:49]1)=[O:43])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 66988Octadecyl isocyanateHCID 23299350HCID 23299350, compound

Product 1

HCID 53858779HCID 53858779, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Triethylamine (0.41 ml) and octadecyl isocyanate (0.91 ml) were added to a solution of 2-[2-(hydroxymethyl)-4,5-dimethoxyphenyl]-1-(4-methylpiperazinyl)-1-ethanone (0.82 g) in dichloromethane (8.5 ml) at room temperature. After being stirred for 15 hours, resulting insoluble materials were filtrated out under a vacuum and washed with chloroform. A mixture of the filtrate and chloroform used for washing was washed with saturated sodium hydrogencarbonate aqueous solution and saturated brine successively, dried over sodium sulfate anhydride, and then concentrated. The residue was purified by silica gel column chromatography (silica gel 50 g, chloroform:methanol=50:1-30:1), thereby yielding 0.83 g of the aimed compound as light brown solid.

Workup

  1. customresulting insoluble materials
  2. filtrationwere filtrated out under a vacuum
  3. washwashed with chloroform
  4. additionA mixture of the filtrate and chloroform
  5. washfor washing
  6. washwas washed with saturated sodium hydrogencarbonate aqueous solution and saturated brine successively
  7. dry with materialdried over sodium sulfate anhydride
  8. concentrationconcentrated
  9. customThe residue was purified by silica gel column chromatography (silica gel 50 g, chloroform:methanol=50:1-30:1)

Sources & evidence

ORD record
ord-40b87eb8c68a4e648c5447edf501be2d
Source dataset
uspto-grants-2000_09
Patent number
US06114325

Reaction notes

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