ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

2-Thiocresol → 2-methylphenyl 2-methyl-N-phenyl-3-(phenylthio)-2-propenimidothioate

HRID 2061011
ノート
印刷プレビュー

反応式

HRID 2061011 の反応式
[CH3:1]/[C:2](=[CH:12]\[S:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)/[C:3]([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=O.S(Cl)(Cl)=O.[CH3:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[SH:31].[H-].[Na+]>CN(C=O)C.O.C1(C)C=CC=CC=1>[CH3:1][C:2](=[CH:12][S:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:3]([S:31][C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=1[CH3:24])=[N:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 87122-ThiocresolHCID 24386Thionyl ChlorideHCID 24758Sodium hydrideHCID 59498330(E)-2-methyl-N-phenyl-3-(phenylthio)-2-propenamide

生成物 1

HCID 675434062-methylphenyl 2-methyl-N-phenyl-3-(phenylthio)-2-propenimidothioate収率 82.5%

試薬・触媒・溶媒 4

HCID 6228
Dimethylformamide
触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒
HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

A mixture of 0.5 g (1.85 mmol) of (E)-2-methyl-N-phenyl-3-(phenylthio)-2-propenamide, 0.4 ml of thionyl chloride, 5 mg of DMF, and 10 ml of toluene was refluxed for 1 hour and then concentrated. The residue was dissolved in 5 ml of DMF and cooled to 0° C. To a solution of 277 mg (2.23 mmol) of 2-methylthiophenol in 5 ml of DMF was added 90 mg of sodium hydride (60% in oil) under ice cooling and stirred for 5 minutes. The solution was added portionwise to the above-described DMF solution of the residue under ice cooling and stirred at room temperature for 1 hour. The reaction mixture was poured into water and extracted with tert-butyl methyl ether (three times). The combined organic layer was washed sequentially with water and a saturated NaCl solution, dried over anhydrous MgSO4, and concentrated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=20/1) to obtain 573 mg of 2-methylphenyl 2-methyl-N-phenyl-3-(phenylthio)-2-propenimidothioate (hereinafter referred to as the present compound 21).

後処理

  1. temperaturewas refluxed for 1 hour
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in 5 ml of DMF
  4. stirringstirred at room temperature for 1 hour
  5. extractionextracted with tert-butyl methyl ether (three times)
  6. washThe combined organic layer was washed sequentially with water
  7. dry with materiala saturated NaCl solution, dried over anhydrous MgSO4
  8. concentrationconcentrated
  9. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=20/1)

出典と根拠

ORDレコード
ord-d1475a81b191440fb986fcb2204ccfb1
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08278473B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート