Pyridine → HCID 178474481、化合物

HRID 275037

反応式

HRID 275037 の反応式
N1C=CC=CC=1.[Cl:7][C:8]1[C:14]([CH3:15])=[CH:13][CH:12]=[C:11]([Cl:16])[C:9]=1[NH2:10].[C:17]([NH:20][C:21]1[NH:25][N:24]=[C:23]([S:26](Cl)(=[O:28])=[O:27])[N:22]=1)(=[O:19])[CH3:18].[OH-].[Na+]>C(Cl)Cl>[Cl:7][C:8]1[C:14]([CH3:15])=[CH:13][CH:12]=[C:11]([Cl:16])[C:9]=1[NH:10][S:26]([C:23]1[N:22]=[C:21]([NH:20][C:17](=[O:19])[CH3:18])[NH:25][N:24]=1)(=[O:27])=[O:28]

参加物

6

反応物 4

HCID 1049PyridineHCID 14798Sodium HydroxideHCID 1165292,6-Dichloro-3-methylanilineHCID 178474479HCID 178474479、化合物

生成物 1

HCID 178474481HCID 178474481、化合物収率 60%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A 250 ml, 1-necked flask equipped with a magnetic stirrer and filled with nitrogen gas was charged with 15 ml of dry pyridine and 8.8 g (0.05 mole) of 2,6-dichloro-3-methylaniline. To the stirred solution was added 11.3 g (0.05 mole) of crude 5-acetylamino-3-chlorosulfonyl-1,2,4-triazole over 10-30 minutes. The resulting dark green mixture, which had a mild exotherm during the addition, was heated to 100°-105° C. with stirring for 3-4 hours. It was then dispersed between a mixture of methylene chloride and dilute aqueous sodium hydroxide and the organic layer was removed. Acidification of the aqueous phase and filtraton and drying of the precipitate that formed gave the title sulfonamide as a tan solid melting at 284° (dec.). The yield was 60 percent of theory. A sample of this compound which was recrystallized from a mixture of methanol and water was a pale ivory powder melting at 285°-285.5° C. (dec.) and had the following elemental analysis: Calc. for C11H11Cl2N5O3S %C, 36.3; %H, 3.04; %N, 19.23 Found 36.3; %H, 3.08; %N, 19.65

後処理

  1. customA 250 ml, 1-necked flask equipped with a magnetic stirrer
  2. additionfilled with nitrogen gas
  3. additionduring the addition
  4. temperaturewas heated to 100°-105° C.
  5. customthe organic layer was removed
  6. customAcidification of the aqueous phase and filtraton and drying of the precipitate
  7. customthat formed

出典と根拠

ORDレコード
ord-d299c22d67304762a2891dfed43843bd
出典データセット
uspto-grants-1995_02
特許番号
US05391759

関連ノート

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