Hydrochloric Acid → HCID 66742899, compound

HRID 1467824Notes

Reaction equation

HRID 1467824 reaction equation
[CH3:1][N:2]1[C:7]2[N:8]([CH3:16])[CH:9]=[C:10]([CH2:11][C:12]([O:14]C)=[O:13])[C:6]=2[C:5](=[O:17])[N:4]([CH3:18])[C:3]1=[O:19].Cl>>[CH3:1][N:2]1[C:7]2[N:8]([CH3:16])[CH:9]=[C:10]([CH2:11][C:12]([OH:14])=[O:13])[C:6]=2[C:5](=[O:17])[N:4]([CH3:18])[C:3]1=[O:19]

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 123561205HCID 123561205, compound

Product 1

HCID 66742899HCID 66742899, compound

Procedure

A mixture of Step 4 intermediate (130 mg, 0.491 mmol) and concentrated hydrochloric acid (4 mL) was heated at 60° C. for 2 h. The excess of hydrochloric acid was evaporated under reduced pressure and the residue obtained was purified by silica gel column chromatography using 5% methanol in chloroform to obtain 94 mg of the product as a white solid; 1H NMR (δ ppm, 300 MHz, DMSO-d6) 3.21 (s, 3H), 3.65-3.72 (m, 8H), 6.29 (s, 1H), 12.62 (br s, 1H); APCI-MS (m/z) 252.38 (M+H)+.

Workup

  1. customThe excess of hydrochloric acid was evaporated under reduced pressure
  2. customthe residue obtained
  3. customwas purified by silica gel column chromatography

Sources & evidence

ORD record
ord-09536db49b4847c8b2f18bf23641cd87
Source dataset
uspto-grants-2015_04
Patent number
US09000159B2

Reaction notes

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