Hydrazine hydrate (1:1) → HCID 14638227, compound

HRID 1253193Notes

Reaction equation

HRID 1253193 reaction equation
O.[NH2:2][NH2:3].Cl[C:5]1[C:10]2[O:11][CH2:12][C:13](=[O:15])[NH:14][C:9]=2[N:8]=[C:7]([CH3:16])[N:6]=1>C(O)CCC>[NH:2]([C:5]1[C:10]2[O:11][CH2:12][C:13](=[O:15])[NH:14][C:9]=2[N:8]=[C:7]([CH3:16])[N:6]=1)[NH2:3]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 608089HCID 608089, compound

Product 1

HCID 14638227HCID 14638227, compoundYield 56.3%

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent2×

Procedure

12.8 ml of 98% hydrazine hydrate dissolved in 40 ml of n-butanol are dropped to a solution of 20 g of 4-chloro-2-methyl-6,7-dihydro-8H-pyrimido[5,4-b][1,4]oxazin-7-one in 320 ml of n-butanol at 117° C. within 30 minutes while stirring. The mixture is stirred for an additional 45 minutes at 117° C., then cooled to room temperature. The precipitate is filtered and washed with water to give 11.66 g (56.3%) of the product, m.p.: 262°-264° C.

Workup

  1. stirringThe mixture is stirred for an additional 45 minutes at 117° C.
  2. filtrationThe precipitate is filtered
  3. washwashed with water

Sources & evidence

ORD record
ord-b50c7c1671484566b3146f1fe3404044
Source dataset
uspto-grants-1988_05
Patent number
US04748175

Reaction notes

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