Acetic Anhydride → HCID 10633310, 화합물

반응식

[NH2:1][C:2]1[C:7]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:6][C:5]([Cl:12])=[CH:4][N:3]=1.[C:13](OC(=O)C)(=O)[CH3:14]>>[Cl:12][C:5]1[CH:4]=[N:3][C:2]2[NH:1][C:13]([CH3:14])=[N:11][S:8](=[O:9])(=[O:10])[C:7]=2[CH:6]=1

참가 물질

반응물 2

HCID 7918Acetic Anhydride

HCID 27796732-Amino-5-chloro-pyridine-3-sulfonic acid amide

생성물 1

HCID 10633310HCID 10633310, 화합물

실험 절차

A mixture of 1 g of 2-amino-5-chloropyridine-3- sulfonamide (Preparation 20) and 10 cm3 of acetic anhydride is brought to reflux for 6 hours. After cooling, the crystals are filtered off, washed with a small amount of acetic anhydride and then with diethyl ether and dried. The crystals are redissolved in 50 cm3 of 0.1N NaOH. The possible insoluble material is removed by filtration. The filtrate, adjusted to a pH of 4 using formic acid, allows crystals to precipitate. They are collected on a filter, washed with water and dried.

후처리

temperatureto reflux for 6 hours
temperatureAfter cooling
filtrationthe crystals are filtered off
washwashed with a small amount of acetic anhydride
dry with materialwith diethyl ether and dried
dissolutionThe crystals are redissolved in 50 cm3 of 0.1N NaOH
customThe possible insoluble material is removed by filtration
customto precipitate
customThey are collected on a filter
washwashed with water
customdried

출처 및 근거

ORD 기록: ord-c361a3ef5cf040938c8c96b9710db92f
출처 데이터셋: uspto-grants-1995_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05459138

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