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

HRID 656308
ノート
印刷プレビュー

反応式

HRID 656308 の反応式
[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
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 24758Sodium hydrideHCID 963933,5-Dimethylpyrazol-1-methanolHCID 148010411-Tert-butyl-4-(isothiocyanatomethyl)benzene

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-242ec50fab224ca091000489e26ecb0a
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08071650B2

反応ノート

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