Hydrazine hydrate (1:1) → MLS002608292

HRID 1768940Notes

Reaction equation

HRID 1768940 reaction equation
[C:1]1([CH:7]2[C:12](=O)[CH:11]=[CH:10][C:9]([CH2:14][CH2:15][CH2:16][C:17](O)=O)=[CH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH2:20].[NH2:21][NH2:22]>C(O)(C)C>[C:1]1([CH:7]2[C:8]([C:9]3[CH:10]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[N:22][NH:21][C:11](=[O:20])[CH2:12]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 67713780HCID 67713780, compound

Product 1

HCID 237489MLS002608292

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Conditions

Temperature
0 °C

Procedure

To a mixture of 3.0 gms of the product from Step A in 25 ml of isopropyl alcohol was added 1.0 ml of hydrazine hydrate and the mixture was refluxed under nitrogen overnight. The reaction was then cooled to 0° C. and filtered and the solids were washed with water and then cold isopropyl alcohol. This afforded 2.32 g of a white solid, mp 221°-223° C. 1H NMR (CDCl3) δ: 2.80 (d, 1H), 3.05 (dd, 1H), 4.50 (d, 1H), 7.1-7.5 (m, 8H), 7.69 (m, 2H), 8.76 (bs, 1H).

Workup

  1. temperaturethe mixture was refluxed under nitrogen overnight
  2. filtrationfiltered
  3. washthe solids were washed with water

Sources & evidence

ORD record
ord-8aade074fba940f99b658017b5e5d437
Source dataset
uspto-grants-1995_01
Patent number
US05380718

Reaction notes

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