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Methanesulfonyl chloride → 4-Pyrimidinemethanol, 2-amino-, 4-methanesulfonate

HRID 1890495
ノート
印刷プレビュー

反応式

HRID 1890495 の反応式
C(N(CC)C(C)C)(C)C.[CH3:10][S:11](Cl)(=[O:13])=[O:12].[NH2:15][C:16]1[N:21]=[C:20]([CH2:22][OH:23])[CH:19]=[CH:18][N:17]=1>O1CCCC1.C(OCC)(=O)C>[NH2:15][C:16]1[N:21]=[C:20]([CH2:22][O:23][S:11]([CH3:10])(=[O:13])=[O:12])[CH:19]=[CH:18][N:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 2004934-Pyrimidinemethanol, 2-amino-

生成物 1

HCID 579711404-Pyrimidinemethanol, 2-amino-, 4-methanesulfonate収率 53%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate
溶媒

実験手順

N,N-Diisopropylethylamine (490 μL, 2.9 mmol) and methanesulfonyl chloride (110 μL, 1.5 mmol) were added to a suspension of 2-amino-4-hydroxymethylpyrimidine (170 mg, 1.3 mmol, Reference Compound No. 4-1) in anhydrous tetrahydrofuran (5.0 mL) under ice-cooling, and the mixture was stirred for 7 hours at room temperature. The reaction mixture was diluted with ethyl acetate (300 mL), washed with water (300 mL), and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, the precipitated solid was filtered off with ethyl acetate, and dried under reduced pressure to give 140 mg of the title Reference Compound as a white solid (Yield: 53%).

後処理

  1. washwashed with water (300 mL)
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. filtrationthe precipitated solid was filtered off with ethyl acetate
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-fc6cbc93284e4f85b5164f68976219c8
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08507485B2

反応ノート

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