Hydrazine hydrate (1:1) → HCID 53751895, compound

HRID 1077412Notes

Reaction equation

HRID 1077412 reaction equation
[C:1]1([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:6]=[CH:5][C:4]([CH:7]=[CH:8][CH2:9][CH2:10]C2C=C3C(=O)NC(=O)C3=CC=2)=[CH:3][CH:2]=1.O.[NH2:29]N>C(O)C>[C:1]1([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:6]=[CH:5][C:4]([CH:7]=[CH:8][CH2:9][CH2:10][NH2:29])=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 86749701HCID 86749701, compound

Product 1

HCID 53751895HCID 53751895, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 280 ml of ethanol, 7.9 g of the product of Stage A and 1.3 ml of hydrazine hydrate was refluxed and then allowed to return to ambient temperature. The precipitate was filtered off and washed with ethanol. After concentration, the product was poured into a 2N hydrochloric acid solution and extraction was carried out with ethyl acetate. The organic phase was washed with water, dried, filtered and concentrated under reduced pressure to obtain 2.89 g of the desired product melting at approximately 188°-194° C.

Workup

  1. temperaturewas refluxed
  2. customto return to ambient temperature
  3. filtrationThe precipitate was filtered off
  4. washwashed with ethanol
  5. concentrationAfter concentration
  6. additionthe product was poured into a 2N hydrochloric acid solution and extraction
  7. washThe organic phase was washed with water
  8. customdried
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-a7f31f8c77694ac986200b6a9c93da26
Source dataset
uspto-grants-1996_08
Patent number
US05543400

Reaction notes

Loading…