Hydrochloric Acid → HCID 69411516, compound

HRID 1592779Notes

Reaction equation

HRID 1592779 reaction equation
C(OC([N:8]1[CH:17]([CH2:18][N:19]([CH:21]([CH2:42][C:43]2[CH:48]=[CH:47][C:46]([Cl:49])=[CH:45][CH:44]=2)[C:22](=[O:41])[N:23]2[CH2:28][CH2:27][N:26]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[CH2:35][N:36]3[CH2:40][CH2:39][CH2:38][CH2:37]3)[CH2:25][CH2:24]2)[CH3:20])[CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:9]1)=O)(C)(C)C.[ClH:50]>O1CCOCC1>[ClH:49].[ClH:50].[ClH:49].[ClH:49].[Cl:49][C:46]1[CH:45]=[CH:44][C:43]([CH2:42][CH:21]([N:19]([CH3:20])[CH2:18][CH:17]2[CH2:16][C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH2:9][NH:8]2)[C:22]([N:23]2[CH2:28][CH2:27][N:26]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[CH2:35][N:36]3[CH2:40][CH2:39][CH2:38][CH2:37]3)[CH2:25][CH2:24]2)=[O:41])=[CH:48][CH:47]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 69410668HCID 69410668, compound

Product 1

HCID 69411516HCID 69411516, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

The material from Step B was taken up in a 4M solution of HCl in dioxane (30 mL). The reaction was stirred at r.t. overnight under nitrogen. The mixture was concentrated to remove dioxane, and the resulting film was triturated with diethyl ether and then concentrated (2×). Trituration with diethyl ether, isolation by suction filtration, and drying at r.t. under vacuum gave about 0.103 g of the final compound as yellow solids (97%). MS (m/z, ES+): 586.3.

Workup

  1. concentrationThe mixture was concentrated
  2. customto remove dioxane
  3. customthe resulting film was triturated with diethyl ether
  4. concentrationconcentrated (2×)
  5. filtrationTrituration with diethyl ether, isolation by suction filtration
  6. customdrying at r.t. under vacuum

Sources & evidence

ORD record
ord-2483e0b0ece349ada771676fa23fbde4
Source dataset
uspto-grants-2007_11
Patent number
US07291619B2

Reaction notes

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