Triphenylphosphine → HCID 117620688、化合物

HRID 626319ノート

反応式

HRID 626319 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].[Br:29][C:30]1([Br:35])[CH2:32][CH:31]1[CH2:33]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>[Br:29][C:30]1([Br:35])[CH2:32][CH:31]1[CH2:33][O:28][C:19]1[CH:20]=[C:21]([CH3:27])[C:22]([N+:24]([O-:26])=[O:25])=[CH:23][C:18]=1[CH3:17]

参加物

7

反応物 5

HCID 11776TriphenylphosphineHCID 2821102,5-Dimethyl-4-nitrophenolHCID 516892Sodium BicarbonateHCID 108897082,2-DibromocyclopropanemethanolHCID 533844152-methoxyethyl N-(2-methoxyethoxycarbonylimino)carbamate

生成物 1

HCID 117620688HCID 117620688、化合物収率 36%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

0.85 g of Bis(2-methoxyethyl) azodicarboxylate was added to a mixture of 0.47 g of 2,5-dimethyl-4-nitrophenol, 0.64 g of (2,2-dibromocyclopropyl)methanol (manufactured according to a reference document (R. Huwyler, A. Al-Dulayymi, M. Neuenschwander, Helv. Chim. Acta 1999, 82, 2336)), 0.87 g of triphenylphosphine and 30 mL of toluene at 0° C., and the mixture was stirred at 80° C. for 5 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 0.38 g of 1-[(2,2-dibromo-cyclopropyl)methoxy]-2,5-dimethyl-4-nitrobenzene.

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-9ffa8bbfa9a24193ab73d42a9ed154b9
出典データセット
uspto-grants-2016_04
特許番号
US09309191B2

反応ノート

読み込み中…