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

HRID 615823
ノート
印刷プレビュー

反応式

HRID 615823 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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°.

後処理

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

出典と根拠

ORDレコード
ord-c2c47e5583744eb2bf804e72f3d29828
出典データセット
uspto-grants-1985_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04501607

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート