Hydrochloride methanol → HCID 21979793, compound

HRID 10493Notes

Reaction equation

HRID 10493 reaction equation
C(OC([NH:8][CH2:9][CH2:10][CH2:11][N:12]([S:20]([C:23]1[CH:32]=[CH:31][CH:30]=[C:29]2[C:24]=1[CH:25]=[CH:26][N:27]=[CH:28]2)(=[O:22])=[O:21])[CH2:13][CH2:14][C:15]1[S:16][CH:17]=[CH:18][CH:19]=1)=O)(C)(C)C.[ClH:33].CO>>[ClH:33].[CH:28]1[C:29]2[C:24](=[C:23]([S:20]([N:12]([CH2:13][CH2:14][C:15]3[S:16][CH:17]=[CH:18][CH:19]=3)[CH2:11][CH2:10][CH2:9][NH2:8])(=[O:22])=[O:21])[CH:32]=[CH:31][CH:30]=2)[CH:25]=[CH:26][N:27]=1

Participants

3

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21979924HCID 21979924, compound

Product 1

HCID 21979793HCID 21979793, compound

Procedure

According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 3 (238 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with methanol (1 ml) and diethyl ether (3 ml). The deposited precipitates were collected by filtration and washed with diethyl ether to obtain the title compound (202 mg) as white powdery solid.

Workup

  1. custom(50° C., 2 hours)
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was added with methanol (1 ml) and diethyl ether (3 ml)
  4. customThe deposited precipitates
  5. filtrationwere collected by filtration
  6. washwashed with diethyl ether

Sources & evidence

ORD record
ord-b5e351201461494c8b84873e8fe9cd2a
Source dataset
uspto-grants-2006_08
Patent number
US07094789B2

Reaction notes

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