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

HRID 1164736

반응식

HRID 1164736 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-68e2f2819e8049869324d22f57c477c2
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04906288

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