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

Sodium hydride → 2-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-2-phenyloxirane

HRID 349717
ノート
印刷プレビュー

反応式

HRID 349717 の反応式
[I-].[CH3:2][S+](C)(C)=O.[H-].[Na+].[F:9][C:10]([F:33])([F:32])[C:11]1[CH:12]=[C:13]([CH:25]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:27]=1)[CH2:14][O:15][CH2:16][C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:18]>CS(C)=O.C(OCC)(=O)C>[F:9][C:10]([F:32])([F:33])[C:11]1[CH:12]=[C:13]([CH:25]=[C:26]([C:28]([F:30])([F:31])[F:29])[CH:27]=1)[CH2:14][O:15][CH2:16][C:17]1([C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH2:2][O:18]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 74498Sulfoxonium, trimethyl-, iodide (1:1)HCID 229606442-{[3,5-Bis(trifluoromethyl)phenyl]methoxy}-1-phenylethan-1-one

生成物 1

HCID 860918462-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-2-phenyloxirane

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

Trimethylsulfoxonium iodide (185 mg, 0.84 mmol) was dissolved in anhydrous dimethylsulfoxide (2 ml). Sodium hydride (60 wt % in mineral oil, 36 mg, 0.9 mmol) was added to the solution and followed by addition of (2-(3,5-bis(trifluoromethyl)benzyloxy)-1-phenylethanone). After stirred for 1 hour, the reaction mixture was diluted with ethyl acetate and washed with brine. The organic layer was dried with magnesium sulfate, concentrated, and the residue was purified by flash chromatography on silica gel to give the desired product. 1H NMR (500 MHz, CHLOROFORM-D) δ ppm 7.76 (s, 1 H) 7.69 (s, 2 H) 7.40–7.45 (m, 2 H) 7.34–7.39 (m, 2 H) 7.30–7.34 (m, 1 H) 4.65–4.72 (m, 2 H) 4.23 (d, J=11.90 Hz, 1 H) 3.79 (d, J=11.60 Hz, 1 H) 3.11 (d, J=5.19 Hz, 1 H) 2.82 (d, J=5.19 Hz, 1 H); LRMS [ESI, MNa+] m/z calcd for C18H14O2F6Na 399.08, found 398.97.

後処理

  1. washwashed with brine
  2. dry with materialThe organic layer was dried with magnesium sulfate
  3. concentrationconcentrated
  4. customthe residue was purified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-bf1c25f6d0bb47d6913da289e20044bc
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07179926B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート