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

Methyl iodide → 2-[(Methylsulfanyl)methyl]-1,1'-biphenyl

HRID 1013148
ノート
印刷プレビュー

反応式

HRID 1013148 の反応式
[C:1]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][SH:8].[CH3:15]I>CO.C[O-].[Na+]>[CH3:15][S:8][CH2:7][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=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

5

反応物 2

HCID 6328Methyl iodideHCID 21610890HCID 21610890、化合物

生成物 1

HCID 230891202-[(Methylsulfanyl)methyl]-1,1'-biphenyl収率 77%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 10942334Sodium Methoxide溶媒

反応条件

温度
60 °C

実験手順

A mixture of biphenyl-2-yl-methanethiol (4 g, 20 mmol) in methanol (27 mL) and sodium methoxide in methanol (0.5 M, 40 mL) was heated at 60° C. for 0.5 h, cooled, treated with methyl iodide (3.7 mL, 60 mmol) and re-heated at 60° C. for 0.5 h. After cooling to room temperature, the reaction mixture was quenched with ice-water, acidified (pH˜2) and extracted with ethyl acetate (3×50 mL). Combined organic layer was washed with water (1×50 mL) and brine (1×50 mL), dried (MgSO4), and concentrated to give a crude product that was passed through a bed of silica (solvent: ethyl acetate) to give 3.3 g of 2-methylsulfanylmethyl-biphenyl (yellow oil) that was directly used in the next step.

後処理

  1. temperaturecooled
  2. temperaturere-heated at 60° C. for 0.5 h
  3. temperatureAfter cooling to room temperature
  4. customthe reaction mixture was quenched with ice-water
  5. extractionextracted with ethyl acetate (3×50 mL)
  6. washCombined organic layer was washed with water (1×50 mL) and brine (1×50 mL)
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated
  9. customto give a crude product that

出典と根拠

ORDレコード
ord-e3aa70915ad8463ebf2b18ee2138c9e0
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07981907B2

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