1,2-Diazinane → 2-Chloro-4-fluoro-5-(1-hexahydropyridazinylthiocarbonylamino)-thiobenzoic acid (methoxycarbonylmethyl) ester

HRID 1033217ノート

反応式

HRID 1033217 の反応式
[CH3:1][O:2][C:3]([CH2:5][O:6][C:7](=[S:19])[C:8]1[CH:13]=[C:12]([N:14]=[C:15]=[S:16])[C:11]([F:17])=[CH:10][C:9]=1[Cl:18])=[O:4].[NH:20]1[CH2:25][CH2:24][CH2:23][CH2:22][NH:21]1>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]([CH2:5][O:6][C:7](=[S:19])[C:8]1[CH:13]=[C:12]([NH:14][C:15]([N:20]2[CH2:25][CH2:24][CH2:23][CH2:22][NH:21]2)=[S:16])[C:11]([F:17])=[CH:10][C:9]=1[Cl:18])=[O:4]

参加物

4

反応物 2

HCID 1363341,2-DiazinaneHCID 538361362-Chloro-4-fluoro-5-isothiocyanatothiobenzoic acid (methoxycarbonylmethyl) ester

生成物 1

HCID 867478262-Chloro-4-fluoro-5-(1-hexahydropyridazinylthiocarbonylamino)-thiobenzoic acid (methoxycarbonylmethyl) ester収率 72.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

A solution of 4.8 g of the resulting 2-chloro-4-fluoro-5-isothiocyanatothiobenzoic acid (methoxycarbonylmethyl) ester in 50 ml of toluene is added dropwise, with stirring, at from 20° to 250° C. to a solution of 1.4 g of hexahydropyridazine in 20 ml of toluene. The batch is then stirred for a further 8 hours at room temperature and is then concentrated by evaporation in vacuo to yield 4.4 g of 2-chloro-4-fluoro-5-(1-hexahydropyridazinylthiocarbonylamino)-thiobenzoic acid (methoxycarbonylmethyl) ester in resinous form.

後処理

  1. concentrationis then concentrated by evaporation in vacuo

出典と根拠

ORDレコード
ord-64ba59b276a6441da47b64ea01800fa4
出典データセット
uspto-grants-1994_05
特許番号
US05310722

反応ノート

読み込み中…