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Hydrochloric Acid → N-(n-butyl)sulfonylurea

HRID 1702527
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HRID 1702527 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8110Butyl isocyanateHCID 11430Potassium CarbonateHCID 13064551Methyl 2-(2-sulfamoylphenyl)acetate

생성물 1

HCID 21473173N-(n-butyl)sulfonylurea수율 135%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

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.).

후처리

  1. temperaturerefluxed for three hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationThe product was filtered
  4. washwashed
  5. customdried
  6. customThe crude product was recrystallized from 1-chlorobutane

출처 및 근거

ORD 기록
ord-10c6fdd59b994806976bd5eca342d21e
출처 데이터셋
uspto-grants-1982_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04348219

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