1,4-Dioxane hydrochloride → HCID 10357072, compound

HRID 1696933Notes

Reaction equation

HRID 1696933 reaction equation
C([N:5]1[C:14]2[C:9](=[CH:10][C:11]([Cl:20])=[C:12]([N:15]3[CH2:19][CH2:18][CH2:17][CH2:16]3)[N:13]=2)[C:8](=[O:21])[C:7]([C:22]([O:24]CC)=[O:23])=[CH:6]1)(C)(C)C.Cl.O1CCOCC1>O>[Cl:20][C:11]1[CH:10]=[C:9]2[C:14](=[N:13][C:12]=1[N:15]1[CH2:19][CH2:18][CH2:17][CH2:16]1)[NH:5][CH:6]=[C:7]([C:22]([OH:24])=[O:23])[C:8]2=[O:21]

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 67275181HCID 67275181, compound

Product 1

HCID 10357072HCID 10357072, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A solution of EXAMPLE 80A (160 mg) in 1:1 9M HCl/1,4-dioxane (15 mL) was heated in a sealed tube at 115° C. for 15 minutes and at 95° C. for 24 hours then cooled, diluted with water (20 mL), and filtered. NMR (300 MHz, DMSO-d6) δ 15.25 (s, 1H), 13.11 (br s, 1H), 8.47 (s, 1H), 8.18 (s, 1H), 3.84-3.80 (m, 4H), 1.96-1.91 (m, 4H).

Workup

  1. temperaturethen cooled
  2. filtrationfiltered

Sources & evidence

ORD record
ord-949952a645ce4d8e9b1cbb80673128e7
Source dataset
uspto-grants-2012_04
Patent number
US08163769B2

Reaction notes

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