Hydrochloric Acid → HCID 135800602, compound

HRID 1732414Notes

Reaction equation

HRID 1732414 reaction equation
[NH2:1][C:2]1[NH:3][C:4](=[O:16])[C:5]2[C:11](C)=[CH:10]C(C)=[N:8][N:7]([CH3:14])[C:6]=2[N:15]=1.Cl>CO>[NH2:1][C:2]1[NH:3][C:4](=[O:16])[C:5]2[C:11]([CH3:10])=[N:8][N:7]([CH3:14])[C:6]=2[N:15]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 13577024670311-77-2

Product 1

HCID 135800602HCID 135800602, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 8-amino-1,3,5-trimethyl-1H-pyrimido{4,5-c}-1,2-diazepin-6(7H)-one (219 mg) and N hydrochloric acid (3 ml) was heated using a hot water bath (>85° C.) for 2 hours. During that period a solution formed before crystals gradually began to separate. The mixture stood at room temperature overnight before the straw-coloured crystals were collected, washed with water and dried under vacuum (70° C.) to yield 140 mg (78%) of analytically pure product: mp >300°; nmr (DMSO-d6) δ 2.28(s, 3H), 3.60(s, 3H), 6.52(br s, 2H), 10.30(br s, 1H); uv λ max (CH3OH) 217 nm (ε 26,800), 254(13,000). Mass spectrum (120° C., 70 ev): M, m/e 179, 100%.

Workup

  1. temperaturewas heated
  2. custom(>85° C.)
  3. customfor 2 hours
  4. customDuring that period a solution formed before crystals
  5. customto separate
  6. customwere collected
  7. washwashed with water
  8. customdried under vacuum (70° C.)
  9. customto yield 140 mg (78%) of analytically pure product
  10. customMass spectrum (120° C., 70 ev)

Sources & evidence

ORD record
ord-da5cd1dfb8764487bf9c4947a3dbdd72
Source dataset
uspto-grants-1980_12
Patent number
US04237289

Reaction notes

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