Benzoic acid, 2-(isocyanatosulfonyl)-, methyl ester → 2-[[(2,6-Dimethoxy-5-nitropyrimidin-4-yl)aminocarbonyl]aminosulfonyl]benzoic acid, methyl ester

HRID 4132

反応式

HRID 4132 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-:12])=[O:11])=[C:5]([O:13][CH3:14])[N:4]=1.[C:15]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[S:25]([N:28]=[C:29]=[O:30])(=[O:27])=[O:26])([O:17][CH3:18])=[O:16]>C(Cl)Cl>[CH3:1][O:2][C:3]1[N:8]=[C:7]([NH:9][C:29]([NH:28][S:25]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[C:15]([O:17][CH3:18])=[O:16])(=[O:27])=[O:26])=[O:30])[C:6]([N+:10]([O-:12])=[O:11])=[C:5]([O:13][CH3:14])[N:4]=1

参加物

4

反応物 2

HCID 156281Benzoic acid, 2-(isocyanatosulfonyl)-, methyl esterHCID 2399532,6-Dimethoxy-5-nitropyrimidin-4-amine

生成物 1

HCID 140502032-[[(2,6-Dimethoxy-5-nitropyrimidin-4-yl)aminocarbonyl]aminosulfonyl]benzoic acid, methyl ester収率 90.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 0.2 g (1.0 mmol) of 2,6-dimethoxy-5-nitro-4-pyrimidinamine and 0.6 g (2.4 mmol) of 2-carbomethoxybenzenesulfonyl isocyanate in 15 ml of methylene chloride was stirred at ambient temperature and pressure for 12 hours under anhydrous conditions. The solvent was then evaporated under reduced pressure. The residue was stirred in n-butyl chloride (70 ml). The solid was then collected by filtration, washed with ether and then dried in an oven to afford 0.4 g of the title compound, m.p. 150°-152° dec.

後処理

  1. customThe solvent was then evaporated under reduced pressure
  2. filtrationThe solid was then collected by filtration
  3. washwashed with ether
  4. customdried in an oven

出典と根拠

ORDレコード
ord-9ecd5cb885984a4aae7b8025b84f1e4f
出典データセット
uspto-grants-1988_02
特許番号
US04723991

関連ノート

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