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Sodium hydride → (4-t-butylbenzyl)thiocarbamic acid-O-(3,5-dimethylpyrazol-1-ylmethyl)ester

HRID 656308
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인쇄 미리보기

반응식

HRID 656308 반응식
[CH3:1][C:2]1[CH:6]=[C:5]([CH3:7])[N:4]([CH2:8][OH:9])[N:3]=1.[H-].[Na+].[C:12]([C:16]1[CH:25]=[CH:24][C:19]([CH2:20][N:21]=[C:22]=[S:23])=[CH:18][CH:17]=1)([CH3:15])([CH3:14])[CH3:13]>O1CCCC1>[CH3:1][C:2]1[CH:6]=[C:5]([CH3:7])[N:4]([CH2:8][O:9][C:22](=[S:23])[NH:21][CH2:20][C:19]2[CH:24]=[CH:25][C:16]([C:12]([CH3:14])([CH3:13])[CH3:15])=[CH:17][CH:18]=2)[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 963933,5-Dimethylpyrazol-1-methanolHCID 148010411-Tert-butyl-4-(isothiocyanatomethyl)benzene

생성물 1

HCID 59087970(4-t-butylbenzyl)thiocarbamic acid-O-(3,5-dimethylpyrazol-1-ylmethyl)ester수율 48.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

3,5-dimethylpyrazol-1-methanol 33-3 (200 mg) and sodium hydride (42 mg) were dissolved in anhydrous tetrahydrofuran (20 ml) and the solution was stirred for 1 hour. To the solution was added 4-t-butylbenzylisothiocyanate (330 mg) and the mixture was stirred at room temperature for 12 hours. The resulting mixture was filtered under reduced pressure and the solvent was removed therefrom. The residue was purified by column-chromatography (ethyl acetate/hexane=1/2) to yield the compound 33-4 (253 mg, 48%) as a solid.

후처리

  1. stirringthe mixture was stirred at room temperature for 12 hours
  2. filtrationThe resulting mixture was filtered under reduced pressure
  3. customthe solvent was removed
  4. customThe residue was purified by column-chromatography (ethyl acetate/hexane=1/2)

출처 및 근거

ORD 기록
ord-242ec50fab224ca091000489e26ecb0a
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08071650B2

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