Hydrochloric Acid → HCID 69419423, compound

HRID 1375016Notes

Reaction equation

HRID 1375016 reaction equation
[Si:1]([O:18][C:19]1[CH:20]=[C:21]([CH:40]=[CH:41][C:42]=1[CH3:43])[CH2:22][C@@H:23]1[CH2:28][N:27]([CH2:29][CH2:30][N:31]2[CH2:36][CH2:35][O:34][C@H:33]([CH2:37][O:38][CH3:39])[CH2:32]2)[CH2:26][CH2:25][NH:24]1)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:44].CCCCCC>C(OCC)(=O)C>[ClH:44].[ClH:44].[ClH:44].[Si:1]([O:18][C:19]1[CH:20]=[C:21]([CH:40]=[CH:41][C:42]=1[CH3:43])[CH2:22][C@@H:23]1[CH2:28][N:27]([CH2:29][CH2:30][N:31]2[CH2:36][CH2:35][O:34][C@H:33]([CH2:37][O:38][CH3:39])[CH2:32]2)[CH2:26][CH2:25][NH:24]1)([C:14]([CH3:15])([CH3:16])[CH3:17])([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 8058HexaneHCID 57161951HCID 57161951, compound

Product 1

HCID 69419423HCID 69419423, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

To a solution of (2R)-2-(3-tert-butyldiphenylsilyloxy-4-methylbenzyl)-4-[2-[(2S)-2-(methoxymethyl)morpholino]ethyl]-piperazine (9.38 g) in ethyl acetate (40 ml) was added 4N hydrogen chloride in ethyl acetate (11.7 ml) at 0° C. and then added dropwise hexane (200 ml). After stirring at room temperature for 2 hours, the mixture was cooled at 0° C. The resulting precipitates were collected by filtration, washed with hexane, and dried under reduced pressure to give (2R)-2-(3-tert-butyldiphenylsilyloxy-4-methylbenzyl)-4-[2-[(2S)-2-(methoxymethyl)morpholino]ethyl]piperazine trihydrochloride (10.75 g) as a powder.

Workup

  1. temperaturethe mixture was cooled at 0° C
  2. customThe resulting precipitates
  3. filtrationwere collected by filtration
  4. washwashed with hexane
  5. customdried under reduced pressure

Sources & evidence

ORD record
ord-0ce0ab07be90462190142ed262ccc96d
Source dataset
uspto-grants-2007_01
Patent number
US07166598B2

Reaction notes

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