Diethyl Sulfate → HCID 18413420, compound

HRID 991371Notes

Reaction equation

S(O[CH2:8][CH3:9])(OCC)(=O)=O.[F:10][C:11]1[CH:16]=[CH:15]C(N)=[CH:13][C:12]=1[N+:18]([O-:20])=[O:19].[C:21](=O)([O-])[O-].[Ca+2].[CH3:26][N:27]([CH3:30])C=O>>[CH2:26]([N:27]([CH2:8][CH3:9])[C:30]1[CH:15]=[CH:16][C:11]([F:10])=[C:12]([N+:18]([O-:20])=[O:19])[CH:13]=1)[CH3:21]

Participants

Reactant 4

HCID 6163Diethyl Sulfate

HCID 6228Dimethylformamide

HCID 10112Calcium Carbonate

HCID 677684-Fluoro-3-nitroaniline

Product 1

HCID 18413420HCID 18413420, compound

Conditions

Temperature: 65 °C

Procedure

197 ml (1.5 mol) of diethyl sulphate were run, over 2 hours, with stirring, into a mixture, heated at 65° C., comprising 63.0 g (0.5 mol) of 4-fluoro-3-nitrophenylamine (RN 364-76-1) and 110 g of calcium carbonate in 150 ml of dimethylformamide and then the mixture was heated at 85° C.-90° C. for 2 hours.

Workup

temperaturethe mixture was heated at 85° C.-90° C. for 2 hours

Sources & evidence

ORD record: ord-e3fca6ba8edb462e99644138d494443e
Source dataset: uspto-grants-2002_10
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06464731B1

Reaction notes

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