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

Triphenylphosphine → 4-Methoxy-3-[2-[4-(trifluoromethyl)phenyl]ethoxy]benzaldehyde

HRID 1826090
ノート
印刷プレビュー

反応式

HRID 1826090 の反応式
N(C(OCC)=O)=NC(OCC)=O.[F:13][C:14]([F:25])([F:24])[C:15]1[CH:20]=[CH:19][C:18]([CH2:21][CH2:22][OH:23])=[CH:17][CH:16]=1.[O:26]=[CH:27][C:28]1[CH:36]=[CH:35][C:32]([O:33][CH3:34])=[C:30](O)[CH:29]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[CH3:34][O:33][C:32]1[CH:35]=[CH:36][C:28]([CH:27]=[O:26])=[CH:29][C:30]=1[O:23][CH2:22][CH2:21][C:18]1[CH:17]=[CH:16][C:15]([C:14]([F:24])([F:25])[F:13])=[CH:20][CH:19]=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 11776TriphenylphosphineHCID 12127IsovanillinHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 112755102-(4-(Trifluoromethyl)phenyl)ethan-1-ol

生成物 1

HCID 118094914-Methoxy-3-[2-[4-(trifluoromethyl)phenyl]ethoxy]benzaldehyde収率 72.3%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

Under an argon atmosphere, stirring and cooling with ice, diethyl azodicarboxylate (40% toluene solution, 3.80 mL, 8.38 mmol) was added dropwise to a solution of 2-[4-(tri-fluoromethyl)phenyl]ethanol (1.59 g, 8.36 mmol), isovanillin (1.28 g, 8.41 mmol) and triphenylphosphine (2.20 g, 8.39 mmol) in anhydrous tetrahydrofuran (50 mL). After completion of the dropwise addition, the mixture was stirred for 1 hour under cooling with ice, and then allowed to stand overnight at room temperature. The reaction mixture was concentrated and the residue was purified by silica gel column chro-matography (eluent: n-hexane:ethyl acetate=6:1 v/v) to afford 1.96 g (72%) of the title compound as colorless crystals.

後処理

  1. additionAfter completion of the dropwise addition
  2. stirringthe mixture was stirred for 1 hour
  3. temperatureunder cooling with ice
  4. concentrationThe reaction mixture was concentrated
  5. customthe residue was purified by silica gel column chro-matography (eluent: n-hexane:ethyl acetate=6:1 v/v)

出典と根拠

ORDレコード
ord-dfee7d1c0db24aa68d2005667405d409
出典データセット
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07049342B2

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