Hydrochloric Acid → HCID 21487306, compound

HRID 1414394Notes

Reaction equation

O([C:8]1[CH:16]=[C:15]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:14]([S:24](=[O:27])(=[O:26])[NH2:25])=[CH:13][C:9]=1[C:10]([OH:12])=[O:11])C1C=CC=CC=1.[CH3:28][O:29][C:30]1[CH:37]=[CH:36][CH:35]=[CH:34][C:31]=1[CH2:32][NH2:33].Cl>C(O)C>[CH3:28][O:29][C:30]1[CH:37]=[CH:36][CH:35]=[CH:34][C:31]=1[CH2:32][NH:33][C:8]1[C:9](=[CH:13][C:14]([S:24](=[O:26])(=[O:27])[NH2:25])=[C:15]([O:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:16]=1)[C:10]([OH:12])=[O:11]

Participants

Conditions

Temperature: 80 °C

Procedure

43 g of 2,4-diphenoxy-5-sulfamoyl-benzoic acid (0.1 mol) prepared according to Example 1 (c) were stirred with 80 ml of 2-methoxybenzylamine for 3.5 hours at 140° C. The almost colorless reaction solution which, had been cooled to about 80° C, was then diluted with 150 ml of ethanol, and the solution was introduced while stirring into 1.0 l of 1N hydrochloric acid at room temperature. The reaction product, which had precipitated in crystals, was suction-filtered and washed with water and then boiled up for a short time with 0.3 l of ethanol, during which the major part of it remained undissolved. After cooling to room temperature, it was suction-filtered and washed with ethanol and finally dried on a steam bath.

Workup

additionthe solution was introduced
customThe reaction product, which had precipitated in crystals
filtrationwas suction-filtered
washwashed with water
temperatureAfter cooling to room temperature
filtrationit was suction-filtered
washwashed with ethanol
customfinally dried on a steam bath

Sources & evidence

ORD record: ord-b3c389bebe894e7c959fe5099f80df85
Source dataset: uspto-grants-1977_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04001284

Reaction notes

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