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2-(Dimethylsulfamoyl)benzene-1-sulfonyl isocyanate → N'-[(4-methoxy-6-methylpyrimidin-2-yl)methylaminocarbonyl]-N,N-dimethyl-1,2-benzenedisulfonamide

HRID 1285086
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HRID 1285086 반응식
[NH2:1][CH2:2][C:3]1[N:8]=[C:7]([CH3:9])[CH:6]=[C:5]([O:10][CH3:11])[N:4]=1.[CH3:12][N:13]([CH3:29])[S:14]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[S:23]([N:26]=[C:27]=[O:28])(=[O:25])=[O:24])(=[O:16])=[O:15]>C(Cl)Cl>[CH3:11][O:10][C:5]1[CH:6]=[C:7]([CH3:9])[N:8]=[C:3]([CH2:2][NH:1][C:27]([NH:26][S:23]([C:18]2[C:17]([S:14]([N:13]([CH3:29])[CH3:12])(=[O:16])=[O:15])=[CH:22][CH:21]=[CH:20][CH:19]=2)(=[O:25])=[O:24])=[O:28])[N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 133926792-(Dimethylsulfamoyl)benzene-1-sulfonyl isocyanateHCID 13392683(4-Methoxy-6-methylpyrimidin-2-YL)methanamine

생성물 1

HCID 13392684N'-[(4-methoxy-6-methylpyrimidin-2-yl)methylaminocarbonyl]-N,N-dimethyl-1,2-benzenedisulfonamide수율 49.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The product from Example 9 (0.90 g) was added in a steady stream to a stirred solution of 2.3 g of 2-(N,N-dimethylsulfamoyl)benzenesulfonyl isocyanate in 20 ml dry methylene chloride at room temperature. The reaction solution was stirred for an additional 18 hours and the solvent was removed in vacuo. The resulting yellow foam was stirred with 1-chlorobutane for ca. one hour. The mixture was filtered and the collected solids dried to yield 1.3 g of N'-[(4-methoxy-6-methylpyrimidin-2-yl)methylaminocarbonyl]-N,N-dimethyl-1,2-benzenedisulfonamide, m.p. 153°-156° C., as a light yellow solid.

후처리

  1. customthe solvent was removed in vacuo
  2. stirringThe resulting yellow foam was stirred with 1-chlorobutane for ca. one hour
  3. filtrationThe mixture was filtered
  4. customthe collected solids dried

출처 및 근거

ORD 기록
ord-f75540589522422f99cd7e52a4e8646a
출처 데이터셋
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04565567

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