Diethyl Ether → HCID 131715852, compound

HRID 2292379Notes

Reaction equation

HRID 2292379 reaction equation
[OH:1][C:2]1[C:18]([OH:19])=[CH:17][CH:16]=[CH:15][C:3]=1[C:4]([N:6](C(OC(C)(C)C)=O)[NH2:7])=[O:5].C(OCC)C.[F:25][C:26]([F:31])([F:30])[C:27]([OH:29])=[O:28].C1(OC)C=CC=CC=1>>[F:25][C:26]([F:31])([F:30])[C:27]([OH:29])=[O:28].[OH:1][C:2]1[C:18]([OH:19])=[CH:17][CH:16]=[CH:15][C:3]=1[C:4]([NH:6][NH2:7])=[O:5]

Participants

4

Reactant 3

HCID 3283Diethyl EtherHCID 66633105Anisole trifluoroacetic acidHCID 86742714HCID 86742714, compound

Product 1

HCID 131715852HCID 131715852, compound

Procedure

(2,3-Dihydroxybenzoyl)hydrazine carboxylic acid, t-butyl ester (17 g) was dissolved in 50 ml of trifluoroacetic acid/anisole (4:1) at 0° C. and stirred for 30 minutes. Diethyl ether (200 ml) was added, and (2,3-dihydroxybenzoyl)hydrazine, trifluoroacetate salt crystallized from the solution. After washing with ether and drying over silica gel, 17.2 g of (2,3-dihydroxybenzoyl)hydrazine, trifluoroacetate salt were obtained as beige, fine crystals; melting point 212° C.

Workup

  1. custom(2,3-dihydroxybenzoyl)hydrazine, trifluoroacetate salt crystallized from the solution
  2. washAfter washing with ether
  3. customdrying over silica gel

Sources & evidence

ORD record
ord-d9e63316d790467cb0a824f3117b9ce7
Source dataset
uspto-grants-1989_01
Patent number
US04801705

Reaction notes

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