Hydrochloride methanol → HCID 21979812, compound

HRID 10494Notes

Reaction equation

HRID 10494 reaction equation
C(OC([NH:8][CH2:9][CH2:10][CH2:11][N:12]([S:23]([C:26]1[CH:35]=[CH:34][CH:33]=[C:32]2[C:27]=1[CH:28]=[CH:29][N:30]=[CH:31]2)(=[O:25])=[O:24])[CH2:13][CH2:14][CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=O)(C)(C)C.[ClH:36].CO>>[ClH:36].[CH:31]1[C:32]2[C:27](=[C:26]([S:23]([N:12]([CH2:13][CH2:14][CH2:15][CH2:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[CH2:11][CH2:10][CH2:9][NH2:8])(=[O:24])=[O:25])[CH:35]=[CH:34][CH:33]=2)[CH:28]=[CH:29][N:30]=1

Participants

3

Procedure

According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 6 (249 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 (188 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-40e9753b7e624fac9a959e0125d91815
Source dataset
uspto-grants-2006_08
Patent number
US07094789B2

Reaction notes

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