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

tert-Butanol → HCID 86711936、化合物

HRID 1475244
ノート
印刷プレビュー

反応式

HRID 1475244 の反応式
[CH:1]([C:3]1[CH:4]=[C:5]([CH2:9][N:10]2[C:14]([CH3:15])=[N:13][C:12]([C:16]3[O:20][N:19]=[C:18]([C:21]4[CH:26]=[CH:25][C:24]([O:27][C:28]([F:31])([F:30])[F:29])=[CH:23][CH:22]=4)[N:17]=3)=[N:11]2)[CH:6]=CC=1)=C.C[N+]1([O-])CC[O:36]CC1.C[C:41]([OH:44])([CH3:43])[CH3:42]>O.O=[Os](=O)(=O)=O>[CH3:15][C:14]1[N:10]([CH2:9][C:5]2[CH:6]=[C:42]([CH:41]([OH:44])[CH2:43][OH:36])[CH:1]=[CH:3][CH:4]=2)[N:11]=[C:12]([C:16]2[O:20][N:19]=[C:18]([C:21]3[CH:26]=[CH:25][C:24]([O:27][C:28]([F:31])([F:30])[F:29])=[CH:23][CH:22]=3)[N:17]=2)[N:13]=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 6386tert-ButanolHCID 82029Methyl morpholine oxideHCID 86711935HCID 86711935、化合物

生成物 1

HCID 86711936HCID 86711936、化合物

試薬・触媒・溶媒 2

HCID 30318Osmium Tetroxide触媒HCID 962Water溶媒

実験手順

To a solution of 5-(5-methyl-1-(3-vinylbenzyl)-1H-1,2,4-triazol-3-yl)-3-(4-(trifluoromethoxy)phenyl)-1,2,4-oxadiazole (Example 84; 110 mg, 0.26 mmol) in t-BuOH (5 mL), were added N-methylmorpholine-N-oxide (152 mg, 1.3 mmol) and OsO4 (10 mg, 0.04 mmol). The reaction mixture was stirred at RT for 24 h, diluted with H2O (20 mL) and extracted with EtOAc (2×10 mL). The combined organic layers were washed with H2O (10 mL) and brine (10 mL), dried over Na2SO4, filtered and concentrated under reduced pressure; the residue was purified by prep-HPLC (10% to 40% MeCN/H2O containing 0.1% trifluoroacetic acid) to give the title compound as a white solid; MS (ES+) C21H18F3N5O4 requires: 461. found: 462 [M+H]+; 1H-NMR (500 MHz, DMSO-d6) δ 8.23 (d, J=8.5 Hz, 2H), 7.61 (d, J=8.5 Hz, 2H), 7.33-7.30 (m, 3H), 7.17 (d, J=7 Hz, 1H), 5.56 (s, 2H), 4.54-4.51 (m, 1H), 3.44-3.40 (m, 4H), 2.57 (s, 3H).

後処理

  1. extractionextracted with EtOAc (2×10 mL)
  2. washThe combined organic layers were washed with H2O (10 mL) and brine (10 mL)
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customthe residue was purified by prep-HPLC (10% to 40% MeCN/H2O containing 0.1% trifluoroacetic acid)

出典と根拠

ORDレコード
ord-cd6f57ae29a543d5bcb43fb025f940cd
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09018380B2

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