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

HRID 1252223
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HRID 1252223 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

HCID 540539623-(p-Nitrobenzyloxycarbonyl)aminomethylbenzyl alcohol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7822ed32ed3a4e20ab8061e3bff0feaf
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04742052

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