Hydrogen chloride-ethyl acetate → HCID 86755372, compound

HRID 1106662Notes

Reaction equation

HRID 1106662 reaction equation
[ClH:1].C(OCC)(=O)C.[CH3:8][N:9]([CH3:46])[CH2:10][CH2:11][CH2:12][N:13]([O:16][CH2:17][CH2:18][CH:19]1[CH2:24][CH2:23][CH2:22][CH2:21][N:20]1[C:25](=[O:45])[NH:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])[CH:14]=[O:15]>C(OCC)(=O)C>[ClH:1].[CH3:46][N:9]([CH3:8])[CH2:10][CH2:11][CH2:12][N:13]([O:16][CH2:17][CH2:18][CH:19]1[CH2:24][CH2:23][CH2:22][CH2:21][N:20]1[C:25](=[O:45])[NH:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])[CH:14]=[O:15]

Participants

4

Procedure

4N Hydrochloric acid/ethyl acetate solution (5.5 ml) was added to a solution of N-[3-(dimethylamino)propyl]-{2-[1-(N-octadecylcarbamoyl)-2-piperidyl]ethoxy}formamide (8.37 g) in ethyl acetate (252 ml) under argon gas atmosphere while being cooled with ice. The solution was stirred for 1.5 hours at room temperature. The deposited crystals were collected by filtration under a vacuum and was recrystallized with ethyl acetate, thereby yielding the entitled compound (8.12 g) as white crystal.

Workup

  1. temperaturewhile being cooled with ice
  2. filtrationThe deposited crystals were collected by filtration under a vacuum
  3. customwas recrystallized with ethyl acetate

Sources & evidence

ORD record
ord-12d6d74b1d064aa989502b0e02fabc14
Source dataset
uspto-grants-2000_05
Patent number
US06057337

Reaction notes

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