Ammonia → HCID 178439841, compound

HRID 568819Notes

Reaction equation

HRID 568819 reaction equation
[CH2:1]([C:4]1[NH:5][C:6]2[CH:12]=[C:11]3[NH:13][C:14](=[O:22])[C:15](C(OCC)=O)([CH3:16])[C:10]3=[CH:9][C:7]=2[N:8]=1)[CH2:2][CH3:3].S(=O)(=O)(O)O.N>>[CH2:1]([C:4]1[NH:5][C:6]2[CH:12]=[C:11]3[NH:13][C:14](=[O:22])[CH:15]([CH3:16])[C:10]3=[CH:9][C:7]=2[N:8]=1)[CH2:2][CH3:3]

Participants

4

Procedure

1.50 g. (4.9 mmole) of the compound prepared in Example 10 is stirred in 30 ml. 60% sulphuric acid for 1 hour at 60° C. bath temperature, then poured on to ice, neutralised with 2N aqueous ammonia solution and the precipitated product is filtered off with suction and the residue crystallised from ethyl acetate/methanol. There is obtained 0.70 g. (62% of theory) of the title compound; m.p. 235°-238° C.

Workup

  1. additionpoured on to ice
  2. filtrationthe precipitated product is filtered off with suction
  3. customthe residue crystallised from ethyl acetate/methanol
  4. customThere is obtained 0.70 g

Sources & evidence

ORD record
ord-8f4172160fe34fab90456ce516185ef4
Source dataset
uspto-grants-1988_03
Patent number
US04730003

Reaction notes

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