Hydrochloric Acid → HCID 18953858, compound

HRID 1491875Notes

Reaction equation

HRID 1491875 reaction equation
[ClH:1].C(OC([NH:9][CH2:10][C:11]([NH:13][CH2:14][C:15]1[S:16][CH:17]=[C:18]([C:20]2[N:21]=[C:22]([N:25]=[C:26]([NH2:28])[NH2:27])[S:23][CH:24]=2)[N:19]=1)=[O:12])=O)(C)(C)C>O1CCOCC1.CO>[ClH:1].[ClH:1].[NH2:9][CH2:10][C:11]([NH:13][CH2:14][C:15]1[S:16][CH:17]=[C:18]([C:20]2[N:21]=[C:22]([N:25]=[C:26]([NH2:28])[NH2:27])[S:23][CH:24]=2)[N:19]=1)=[O:12]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 18953798HCID 18953798, compound

Product 1

HCID 18953858HCID 18953858, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 312751,4-DioxaneSolvent

Procedure

A solution of hydrogen chloride in dioxane (4N, 5 ml) was added slowly to a suspension of 4-(2-t-butoxycarbonylaminoacetylaminomethylthiazol-4-yl)-2-(diaminomethyleneamino)thiazole (1.0 g) in methanol (5 ml) with cooling on an ice-water bath. The mixture was stirred for 24 hours with cooling on an ice-water bath. The resulting precipitate was collected by filtration. Recrystallization from a mixture of methanol and diisopropyl ether afforded 4-(2-aminoacetylaminomethylthiazol-4-yl)-2-(diaminomethyleneamino)thiazole dihydrochloride (0.58 g).

Workup

  1. temperaturewith cooling on an ice-water bath
  2. temperaturewith cooling on an ice-water bath
  3. filtrationThe resulting precipitate was collected by filtration
  4. customRecrystallization
  5. additionfrom a mixture of methanol and diisopropyl ether

Sources & evidence

ORD record
ord-fb59fe726c394020bfe17f148b1488b9
Source dataset
uspto-grants-1994_12
Patent number
US05371097

Reaction notes

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