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'-(2-Methoxyethoxymethoxy)-[1,1';3',1"]terphenyl-5'-carboxylic acid

HRID 1067314
ノート
印刷プレビュー

反応式

HRID 1067314 の反応式
[OH-:1].[Na+].[CH3:3][O:4][CH2:5][CH2:6][O:7][CH2:8][O:9][C:10]1[C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:14][C:13]([CH:22]=[O:23])=[CH:12][C:11]=1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>O.C1COCC1.[Ag-]=O>[CH3:3][O:4][CH2:5][CH2:6][O:7][CH2:8][O:9][C:10]1[C:11]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)=[CH:12][C:13]([C:22]([OH:1])=[O:23])=[CH:14][C:15]=1[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=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

6

反応物 2

HCID 14798Sodium Hydroxide2 回HCID 222375093,5-Diphenyl-4-[(2-methoxyethoxy)methoxy]-benzaldehyde

生成物 1

HCID 234456652'-(2-Methoxyethoxymethoxy)-[1,1';3',1"]terphenyl-5'-carboxylic acid収率 93%

試薬・触媒・溶媒 3

HCID 178418778HCID 178418778、化合物触媒2 回HCID 962Water溶媒2 回
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
50 °C

実験手順

At ambient temperature, to a stirred mixture of silver (I) oxide (0.570 g, 2.46 mmol) in H2O (9.8 mL) was added NaOH (0.983 g, 24.6 mmol) and the reaction was heated at 50° C. After 0.5 h, to the reaction was added a solution of 2′-(2-methoxyethoxymethoxy)-[1,1′;3′,1″]terphenyl-5′-carbaldehyde (1.78 g, 4.92 mmol) in THF (9.8 mL) and the reaction was heated at 90° C. for 1h. To the reaction was added silver (I) oxide (0.570 g, 2.46 mmol), NaOH (0.983 g, 24.6 mmol) and H2O (10.0 mL). The reaction was heated at 90° C. for 16 h. The reaction was filtered through a celite pad, rinsing with hot H2O (3×). The filtrate was washed with ether (3×), acidified with 2N HCl (pH 2) and extracted with EtOAc. The organic extracts were dried (MgSO4) and concentrated to give 1.73 g (93%) of the title compound. 1H NMR (DMSO-d6) δ2.77-2.80 (m, 2H), 2.88-2.91 (m, 2H), 3.01 (s, 3H), 4.39 (s, 2H), 7.39-7.52 (m, 6H), 7.59-7.62 (m, 4H), 7.89 (s, 2H), 13.07 (s, 1H).

後処理

  1. temperaturethe reaction was heated at 90° C. for 1h
  2. temperatureThe reaction was heated at 90° C. for 16 h
  3. filtrationThe reaction was filtered through a celite pad
  4. washrinsing with hot H2O (3×)
  5. washThe filtrate was washed with ether (3×)
  6. extractionextracted with EtOAc
  7. dry with materialThe organic extracts were dried (MgSO4)
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-a11fd29ee47b47a0922a3a4c6d14573e
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06248764B1

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