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Triphenylphosphine → 2,5-Dimethyl-4-nitro-1-[(2,2,3,3-tetramethylcyclopropyl)methoxy]benzene

HRID 626318
ノート
印刷プレビュー

反応式

HRID 626318 の反応式
N(C(OCCOC)=O)=NC(OCCOC)=O.[CH3:17][C:18]1[CH:23]=[C:22]([N+:24]([O-:26])=[O:25])[C:21]([CH3:27])=[CH:20][C:19]=1[OH:28].[CH3:29][C:30]1([CH3:37])[C:32]([CH3:34])([CH3:33])[CH:31]1[CH2:35]O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1>[CH3:17][C:18]1[CH:23]=[C:22]([N+:24]([O-:26])=[O:25])[C:21]([CH3:27])=[CH:20][C:19]=1[O:28][CH2:35][CH:31]1[C:32]([CH3:34])([CH3:33])[C:30]1([CH3:37])[CH3:29]
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

7

反応物 5

HCID 11776TriphenylphosphineHCID 2821102,5-Dimethyl-4-nitrophenolHCID 516892Sodium BicarbonateHCID 5441792,2,3,3-TetramethylcyclopropanemethanolHCID 533844152-methoxyethyl N-(2-methoxyethoxycarbonylimino)carbamate

生成物 1

HCID 1176205752,5-Dimethyl-4-nitro-1-[(2,2,3,3-tetramethylcyclopropyl)methoxy]benzene
収率 8.4%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

1.97 g of Bis(2-methoxyethyl) azodicarboxylate was added to a mixture of 1.08 g of 2,5-dimethyl-4-nitrophenol, 0.83 g of (2,2,3,3-tetramethylcyclopropyl)methanol, 2.04 g of triphenylphosphine and 100 mL of toluene at 0° C., and the mixture was stirred at 90° C. for 4 hours. After cooling, a saturated aqueous sodium bicarbonate solution was added, and the mixture was extracted with ethyl acetate, and then the organic layer was washed with water and saturated salt water and dried over anhydrous magnesium sulfate. The resulting residue was subjected to silica gel column chromatography to obtain 0.15 g of 2,5-dimethyl-4-nitro-1-[(2,2,3,3-tetramethylcyclopropyl) methoxy]benzene.

後処理

  1. temperatureAfter cooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. washthe organic layer was washed with water and saturated salt water
  4. dry with materialdried over anhydrous magnesium sulfate

出典と根拠

ORDレコード
ord-23c8524c408f49c9a356b4fac06ecd9e
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09309191B2

反応ノート

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