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Hydrochloride methanol → HCID 178418877, compound

HRID 10559
Notes
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Reaction equation

HRID 10559 reaction equation
C(OC([NH:8][C@H:9]1[CH2:14][CH2:13][C@H:12]([NH:15][C:16]2[CH:25]=[CH:24][CH:23]=[C:22]3[C:17]=2[C:18]([CH3:26])=[CH:19][N:20]=[CH:21]3)[CH2:11][CH2:10]1)=O)(C)(C)C.[ClH:27].CO>>[ClH:27].[CH3:26][C:18]1[C:17]2[C:22](=[CH:23][CH:24]=[CH:25][C:16]=2[NH:15][C@H:12]2[CH2:13][CH2:14][C@H:9]([NH2:8])[CH2:10][CH2:11]2)[CH:21]=[N:20][CH:19]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 2

HCID 21893726Hydrochloride methanolHCID 178418972HCID 178418972, compound

Product 1

HCID 178418877HCID 178418877, compound

Procedure

According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 95 (389 mg) and 10% hydrogen chloride/methanol solution (10 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (2 ml) and diethyl ether (6 ml). The deposited precipitates were collected by filtration and washed with diethyl ether to obtain the title compound (355 mg) as light yellow powdery solid.

Workup

  1. custom(room temperature, 2 hours)
  2. customThe solvent was evaporated under reduced pressure
  3. additionthe residue was added with methanol (2 ml) and diethyl ether (6 ml)
  4. custom
The deposited precipitates
  • filtrationwere collected by filtration
  • washwashed with diethyl ether
  • Sources & evidence

    ORD record
    ord-59ed023d969d467280c5a315d794f41e
    Source dataset
    uspto-grants-2006_08
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US07094789B2

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes