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4,6-Dimethyl-2-(4-nitrobenzyloxycarbonylthio)pyrimidine → 3-(p-Nitrobenzyloxycarbonyl)aminomethylbenzyl alcohol

HRID 1252223
ノート
印刷プレビュー

反応式

HRID 1252223 の反応式
[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH2:7].[N+:11]([C:14]1[CH:32]=[CH:31][C:17]([CH2:18][O:19][C:20](SC2N=C(C)C=C(C)N=2)=[O:21])=[CH:16][CH:15]=1)([O-:13])=[O:12]>O1CCCC1>[N+:11]([C:14]1[CH:15]=[CH:16][C:17]([CH2:18][O:19][C:20]([NH:7][CH2:6][C:5]2[CH:4]=[C:3]([CH:10]=[CH:9][CH:8]=2)[CH2:2][OH:1])=[O:21])=[CH:31][CH:32]=1)([O-:13])=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 135043164,6-Dimethyl-2-(4-nitrobenzyloxycarbonylthio)pyrimidineHCID 21880609[3-(Aminomethyl)phenyl]methanol

生成物 1

HCID 540539623-(p-Nitrobenzyloxycarbonyl)aminomethylbenzyl alcohol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To 3-hydroxymethylbenzylamine (1.37 g) in tetrahydrofuran (30 ml), a solution of S-p-nitrobenzyloxycarbonyl-4,6-dimethyl-2-mercaptopyrimidine (6.2 g) in tetrahydrofuran (20 ml) was added at room temperature, followed by stirring for 1 hours. The resulting precipitates were removed by filtration and the filtrate was diluted with ethyl acetate, washed with water, dried over anhydrous sodium sulfate and evaporated in vacuo to give an oily residue which was then crystallized from diethyl etherdichloromethane to give 3-(p-nitrobenzyloxycarbonyl)aminomethylbenzyl alcohol.

後処理

  1. customThe resulting precipitates
  2. customwere removed by filtration
  3. additionthe filtrate was diluted with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customevaporated in vacuo
  7. customto give an oily residue which
  8. customwas then crystallized from diethyl etherdichloromethane

出典と根拠

ORDレコード
ord-7822ed32ed3a4e20ab8061e3bff0feaf
出典データセット
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04742052

反応ノート

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