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 Hydroxide → 2-triphenylmethoxymethyl-2-propen-1-ol

HRID 931843
ノート
印刷プレビュー

反応式

HRID 931843 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[Al+3].[Cl-].[Cl-].[Cl-].[C:11]1([C:17]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[O:18][CH2:19][C:20](=[CH2:24])[CH2:21]C#N)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[OH-:37].[Na+]>CCOCC>[C:31]1([C:17]([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[O:18][CH2:19][C:20](=[CH2:24])[CH2:21][OH:37])[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=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 4

HCID 14798Sodium HydroxideHCID 6451240Aluminum(III) ChlorideHCID 21226445Aluminium lithium hydrideHCID 57915012HCID 57915012、化合物

生成物 1

HCID 111633262-triphenylmethoxymethyl-2-propen-1-ol収率 65%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether
溶媒
2 回

実験手順

To a solution of LiAlH4 (119 mg; 2.98 mmol) in dry ether (5 mL), AlCl3 (400 mg; 2.94 mmol) was added carefully at 0° C. and the mixture was stirred for 15 min. Then a solution of 12 (829 mg; 2.44 mmol) in dry ether (9 mL) was added and the reaction was stirred at 0° C. for 3 h. After that 10% aqueous NaOH (10 mL) was added to quench the reaction. The organic layer was separated and washed by saturated aqueous NaHCO3 and NaCl respectively, and dried over anhydrous K2CO3. After evaporation of the solvent, the residue was purified by flash column chromatography over silica gel using CH3OH—CH2Cl2 (1:205) as the eluent to afford 10 as colorless oil (545 mg; 65% yield): 1H NMR (400 MHz, CDCl3) δ 7.41-7.48 (m, 6H, six of ArH), 7.26-7.33 (m, 6H, six of ArH), 7.19-7.26 (m, 3H, three of ArH), 5.33 (s, 1H, one of C═CH2), 4.96 (s, 1H, one of C═CH2), 3.53 (s, 2H, Ph3COCH2), 2.70 (m, 2H, CH2CH2NH2) 2.18 (t, J=6.7 Hz, 2H, CH2CH2NH2), 2.06 (br s, 2H, NH2); 13C NMR (100 MHz, CDCl3) δ 143.6, 143.4, 128.1, 127.4, 126.5, 111.3, 86.5, 66.1, 39.8, 37.4; HRMS (FAB+) calcd for C24H26ON (M+H+): 344.2014. found: 344.2017, (11).

後処理

  1. stirringthe reaction was stirred at 0° C. for 3 h
  2. customto quench
  3. customthe reaction
  4. customThe organic layer was separated
  5. washwashed by saturated aqueous NaHCO3 and NaCl respectively
  6. dry with materialdried over anhydrous K2CO3
  7. customAfter evaporation of the solvent
  8. customthe residue was purified by flash column chromatography over silica gel

出典と根拠

ORDレコード
ord-51d1c6eb6c424b7785b25921eee4e54a
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09297042B2

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