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Sodium Hydroxide → Methyl [6-methyl-2-[(2-thienylsulfonyl)aminocarbonylamino]pyrimidin-4-yloxy]acetate

HRID 615823
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HRID 615823 반응식
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH2:9][C:10]([O:12][CH3:13])=[O:11])[CH:5]=[C:4]([CH3:14])[N:3]=1.[S:15]1[CH:19]=[CH:18][CH:17]=[C:16]1[S:20]([N:23]=[C:24]=[O:25])(=[O:22])=[O:21].[OH-].[Na+]>C(Cl)Cl>[CH3:14][C:4]1[N:3]=[C:2]([NH:1][C:24]([NH:23][S:20]([C:16]2[S:15][CH:19]=[CH:18][CH:17]=2)(=[O:21])=[O:22])=[O:25])[N:7]=[C:6]([O:8][CH2:9][C:10]([O:12][CH3:13])=[O:11])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 12875192Thiophene-2-sulfonyl isocyanateHCID 13469547Methyl (2-amino-6-methylpyrimidin-4-yloxy)acetate

생성물 1

HCID 13469548Methyl [6-methyl-2-[(2-thienylsulfonyl)aminocarbonylamino]pyrimidin-4-yloxy]acetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a dry stirred solution of 18 parts of methyl (2-amino-6-methylpyrimidin-4-yloxy)acetate in 300 parts of methylene chloride at ambient temperature was added 20 parts of 2-thiophenesulfonylisocyanate. The solution was allowed to stand for 3 hours and was then poured onto ice. The pH of the aqueous layer was adjusted to 11 with sodium hydroxide solution and the methylene chloride layer was separated therefrom. The aqueous layer was neutralized with aqueous hydrochloric acid and then extracted with methylene chloride. The extract was dried and stripped of solvent to yield 8 parts of methyl [6-methyl-2-[(2-thienylsulfonyl)aminocarbonylamino]pyrimidin-4-yloxy]acetate, m.p. 114°-120°.

후처리

  1. additionwas then poured onto ice
  2. customthe methylene chloride layer was separated
  3. extractionextracted with methylene chloride
  4. customThe extract was dried

출처 및 근거

ORD 기록
ord-c2c47e5583744eb2bf804e72f3d29828
출처 데이터셋
uspto-grants-1985_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04501607

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