Hydrochloric Acid → N-(n-butyl)sulfonylurea
反応式
[NH2:1][S:2]([C:5]1[CH:10]=[CH:9][CH:8]=CC=1CC(OC)=O)(=[O:4])=[O:3].C([N:20]=[C:21]=[O:22])CCC.C(=O)([O-])[O-].[K+].[K+].Cl>C(C(C)=O)C>[CH2:5]([S:2]([NH:1][C:21]([NH2:20])=[O:22])(=[O:3])=[O:4])[CH2:10][CH2:9][CH3:8]参加物
6
実験手順
A mixture of 22.9 g methyl o-aminosulfonylbenzeneacetate, 13.5 g n-butyl isocyanate, 15.2 g potassium carbonate and 250 ml methyl ethyl ketone was stirred and refluxed for three hours. The reaction mixture was cooled, poured into 1250 g of ice-water, and acidified to pH 1.5 with concentrated HCl. The product was filtered, washed and dried. The crude product was recrystallized from 1-chlorobutane to yield 24.3 g of purified N-(n-butyl)sulfonylurea derivative of methyl o-isocyanatosulfonylbenzeneacetate, m.p. 164°-166° (dec.).
後処理
- temperaturerefluxed for three hours
- temperatureThe reaction mixture was cooled
- filtrationThe product was filtered
- washwashed
- customdried
- customThe crude product was recrystallized from 1-chlorobutane
出典と根拠
- ORDレコード
- ord-10c6fdd59b994806976bd5eca342d21e
- 出典データセット
- uspto-grants-1982_09
- 特許番号
- US04348219
反応ノート
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