1,4-Dioxane hydrochloride → HCID 67070371, compound

HRID 2390882Notes

Reaction equation

HRID 2390882 reaction equation
C(OC([NH:8][C@@H:9]([CH:47]([CH3:49])[CH3:48])[C:10]([O:12][CH2:13][N:14]1[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([C:21]2[CH:26]=[C:25](/[CH:27]=[CH:28]/[C:29]3[CH:34]=[CH:33][C:32]([NH:35][S:36]([CH3:39])(=[O:38])=[O:37])=[CH:31][CH:30]=3)[C:24]([O:40][CH3:41])=[C:23]([C:42]([CH3:45])([CH3:44])[CH3:43])[CH:22]=2)[C:15]1=[O:46])=[O:11])=O)(C)(C)C.Cl.O1CCOCC1>C(Cl)Cl>[C:42]([C:23]1[CH:22]=[C:21]([C:16]2[C:15](=[O:46])[N:14]([CH2:13][O:12][C:10](=[O:11])[C@@H:9]([NH2:8])[CH:47]([CH3:48])[CH3:49])[CH:19]=[C:18]([F:20])[CH:17]=2)[CH:26]=[C:25](/[CH:27]=[CH:28]/[C:29]2[CH:34]=[CH:33][C:32]([NH:35][S:36]([CH3:39])(=[O:38])=[O:37])=[CH:31][CH:30]=2)[C:24]=1[O:40][CH3:41])([CH3:43])([CH3:45])[CH3:44]

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 131729968HCID 131729968, compound

Product 1

HCID 67070371HCID 67070371, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

step 3—To a solution of 342 (0.886 g, 1.266 mmol and DCM (10 mL) at RT was added a HCl/dioxane solution (1.899 mL, 7.60 mmol, 4M solution) and the resulting solution stirred at RT for 3 h. The resulting solution was poured into DCM (150 mL) which produced a gummy oil. When the mixture was sonicated a white powder formed which was filtered, washed with DCM and air-dried. The solid was dried under high vacuum to remove all traces of solvent which afforded 698 g of II-7 as a white powder: MS (M+H)=600.

Workup

  1. customproduced a gummy oil
  2. customWhen the mixture was sonicated a white powder
  3. customformed which
  4. filtrationwas filtered
  5. washwashed with DCM
  6. customair-dried
  7. customThe solid was dried under high vacuum
  8. customto remove all traces of solvent which
  9. customafforded 698 g of II-7 as a white powder

Sources & evidence

ORD record
ord-5d7f21aa968d4a01a67793a439425d4e
Source dataset
uspto-grants-2012_09
Patent number
US08273773B2

Reaction notes

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