Diisopropylethylamine → N-diaminomethylene-3-methylsulfonyl-4-(3-pyridyloxy)-6-methylbenzamide

HRID 376866ノート

反応式

HRID 376866 の反応式
[CH3:1][S:2]([C:5]1[CH:6]=[C:7]([C:11]([CH3:21])=[CH:12][C:13]=1[O:14][C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)[C:8](O)=[O:9])(=[O:4])=[O:3].[Cl-].C[N+]1C=CC=CC=1Cl.[Cl-].[NH2:32][C:33]([NH2:35])=[NH2+:34].C(N(C(C)C)C(C)C)C>CN1CCCC1=O>[NH2:34][C:33]([NH2:35])=[N:32][C:8](=[O:9])[C:7]1[C:11]([CH3:21])=[CH:12][C:13]([O:14][C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[C:5]([S:2]([CH3:1])(=[O:4])=[O:3])[CH:6]=1

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 5460839Carbamimidoylazanium ChlorideHCID 117449626-chloro-N-methylpyridinium chlorideHCID 193603313-Methylsulfonyl-4-(3-pyridyloxy)-6-methylbenzoic acid

生成物 1

HCID 10712709N-diaminomethylene-3-methylsulfonyl-4-(3-pyridyloxy)-6-methylbenzamide

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

1.0 g of 3-methylsulfonyl-4-(3-pyridyloxy)-6-methylbenzoic acid [obtainable by reacting 3-methylsulfonyl-4-chloro-6-methylbenzoic acid with 3-hydroxypyridine] is dissolved in 15 ml of 1-methylpyrrolidone, and 0.67 g of 1-methyl-2-chloropyridinium chloride is added to this solution, which is stirred for 15 min. 0.9 g of guanidinium chloride and 2.6 ml of N-ethyldiisopropylamine are then added, and the mixture is stirred at room temperature for one hour. Following customary working-up, N-diaminomethylene-3-methylsulfonyl-4-(3-pyridyloxy)-6-methylbenzamide is obtained, m.p. 221-224°.

後処理

  1. stirringthe mixture is stirred at room temperature for one hour

出典と根拠

ORDレコード
ord-c2ebe1b38c8f4887a8c02cbc90e35665
出典データセット
uspto-grants-2000_02
特許番号
US06022883

反応ノート

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