Triphenylphosphine → [2-(4-Cyanophenyl)ethoxy]-4-methyl-3-nitrobenzene

HRID 325035

反応式

HRID 325035 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10].[C:12]([C:14]1[CH:19]=[CH:18][C:17]([CH2:20][CH2:21]O)=[CH:16][CH:15]=1)#[N:13].CCOC(/N=N/C(OCC)=O)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[C:12]([C:14]1[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][O:8][C:5]2[CH:6]=[CH:7][C:2]([CH3:1])=[C:3]([N+:9]([O-:11])=[O:10])[CH:4]=2)=[CH:16][CH:15]=1)#[N:13]

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 162713-Nitro-p-cresolHCID 28008154-(2-Hydroxyethyl)benzonitrileHCID 5462977Diethyl azodicarboxylate

生成物 1

HCID 22033464[2-(4-Cyanophenyl)ethoxy]-4-methyl-3-nitrobenzene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

4-Methyl-3-nitrophenol (0.765 g; 5.0 mmol), 2-(4-cyanophenyl)ethanol (0.735 g; 5.0 mmol) and diethylazodicarboxylate (0.87 g; 5.0 mmol) were dissolved in THF (20 mL). Triphenylphosphine (1.31 g; 5.0 mmol), dissolved in THF (5 mL), was added and the solution stirred overnight. Evaporation in vacuo and the addition of diethyl ether afforded a yellow solid that was recrystallized from water:acetone (9:1), affording the sub-title compound as yellowish crystals. Yield: 1.04 g (74%).

後処理

  1. additionwas added
  2. customEvaporation in vacuo
  3. additionthe addition of diethyl ether
  4. customafforded a yellow solid
  5. customthat was recrystallized from water:acetone (9:1)

出典と根拠

ORDレコード
ord-d970b539f2dc42ef96a33271cf91092f
出典データセット
uspto-grants-2001_04
特許番号
US06221898B1

関連ノート

読み込み中…