Hydrazine hydrate (1:1) → HCID 53781734, compound

HRID 355506Notes

Reaction equation

HRID 355506 reaction equation
[C:1]([O:9][C@@H:10]1[C@@H:14]([CH2:15][O:16][C:17](=[O:24])[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[O:13][C@@H:12]([N:25]2[C:29]([N:30]3C(=O)C4=CC=CC=C4C3=O)=[C:28]([C:41](=[O:44])[CH2:42][Cl:43])[N:27]=[CH:26]2)[C@H:11]1[F:45])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.NN>ClCCl>[NH2:30][C:29]1[N:25]([C@@H:12]2[O:13][C@H:14]([CH2:15][O:16][C:17](=[O:24])[C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[C@@H:10]([O:9][C:1](=[O:8])[C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C@@H:11]2[F:45])[CH:26]=[N:27][C:28]=1[C:41](=[O:44])[CH2:42][Cl:43]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 54097139HCID 54097139, compound

Product 1

HCID 53781734HCID 53781734, compoundYield 95%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Compound (15) obtained in step (6) above (220 mg) was dissolved in dichloromethane (9 ml), to which was then added hydrazine monohydrate (0.02 ml) under cooling at 0° C., and the resultant mixture was allowed to effect the reaction under stirring at the same temperature for 1 hour to produce the titled compound (16). The reaction solution obtained was filtered and the filtrate was concentrated to leave a solid. The solid was purified by silica gel column chromatography (developer solvent:toluene-ethyl acetate, 1:1), to afford the titled compound (16) as a colorless solid (166 mg). Yield: 95%.

Workup

  1. customthe reaction

Sources & evidence

ORD record
ord-f21f4cbe4a714242be39986973e38357
Source dataset
uspto-grants-1998_11
Patent number
US05831072

Reaction notes

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