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Diethyl Ether → 2-[2-(4,6-Dimethoxypyrimidin-2-yloxy)-6-fluorophenylsulfamoyl]-N-methylacetamide

HRID 743984
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HRID 743984 반응식
[CH3:1][NH2:2].[CH3:3][O:4][C:5]1[CH:10]=[C:9]([O:11][CH3:12])[N:8]=[C:7]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[C:15]=2[NH:21][S:22]([CH2:25][C:26]([O:28]C)=O)(=[O:24])=[O:23])[N:6]=1.C(OCC)C.C(O)(C)C>CO>[CH3:3][O:4][C:5]1[CH:10]=[C:9]([O:11][CH3:12])[N:8]=[C:7]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[C:15]=2[NH:21][S:22]([CH2:25][C:26]([NH:2][CH3:1])=[O:28])(=[O:24])=[O:23])[N:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 3776IsopropanolHCID 6329MethylamineHCID 54135497Methyl [2-(4,6-dimethoxypyrimidin-2-yloxy)-6-fluorophenylsulfamoyl]acetate

생성물 1

HCID 541152332-[2-(4,6-Dimethoxypyrimidin-2-yloxy)-6-fluorophenylsulfamoyl]-N-methylacetamide

시약·촉매·용매 1

HCID 887
Methanol
용매

실험 절차

Methylamine (4.2 g of a 33% solution in industrial methylated spirits) was added to a solution of the product of stage (a) (3 g) in methanol (60 ml) at room temperature. After standing for 23 days, the solution was run down under vacuum at less than 35° C. to give a brown oil. Trituration with a mixture of diethyl ether and isopropanol gave an off-white solid which was dried without heat to give 1.3 g of the desired product, mp 193°-198° C.

후처리

  1. customwas run down under vacuum at less than 35° C.
  2. customto give a brown oil
  3. customgave an off-white solid which
  4. customwas dried
  5. temperaturewithout heat

출처 및 근거

ORD 기록
ord-cd7f04f5e30941738c179d2ee8e27925
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05559081

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